Pub Date : 2016-12-02DOI: 10.12677/JOCR.2016.44013
吴阳, 邢雪建, 邢刘桩, 侯亚东, 杨敬辉, 惠永海
本文以杂多酸–磷钨酸为催化剂，对酰肼与查尔酮的缩合反应进行了研究。经过一系列反应条件的筛选，确立了最佳反应条件，并对底物的普适性进行了考察，得到了一系列高产率的酰腙类目标产物，最高产率达到99%。本反应操作简单，条件温和，为查尔酮酰腙合成提供了一种新的方法。 The condensation of hydrazide with benzylideneacetophenone was studied by using phospho-tungstic acid as catalyst. After a series of reaction conditions, the optimal reaction conditions were established, and the universality of the substrate was investigated. A series of acylhydrazones were obtained with the high yields, up to 99%. The reaction was simple and mild, which provided a new method for the synthesis of chalcone hydrazone.
本文以杂多酸–磷钨酸为催化剂，对酰肼与查尔酮的缩合反应进行了研究。经过一系列反应条件的筛选，确立了最佳反应条件，并对底物的普适性进行了考察，得到了一系列高产率的酰腙类目标产物，最高产率达到99%。本反应操作简单，条件温和，为查尔酮酰腙合成提供了一种新的方法。 The condensation of hydrazide with benzylideneacetophenone was studied by using phospho-tungstic acid as catalyst. After a series of reaction conditions, the optimal reaction conditions were established, and the universality of the substrate was investigated. A series of acylhydrazones were obtained with the high yields, up to 99%. The reaction was simple and mild, which provided a new method for the synthesis of chalcone hydrazone.
{"title":"磷钨酸促进的酰肼与查尔酮缩合反应的研究 Study on the Condensation Reaction of Hydrazide with Benzylideneacetophenone Catalyzed by Phosphotungstic Acid","authors":"吴阳, 邢雪建, 邢刘桩, 侯亚东, 杨敬辉, 惠永海","doi":"10.12677/JOCR.2016.44013","DOIUrl":"https://doi.org/10.12677/JOCR.2016.44013","url":null,"abstract":"本文以杂多酸–磷钨酸为催化剂，对酰肼与查尔酮的缩合反应进行了研究。经过一系列反应条件的筛选，确立了最佳反应条件，并对底物的普适性进行了考察，得到了一系列高产率的酰腙类目标产物，最高产率达到99%。本反应操作简单，条件温和，为查尔酮酰腙合成提供了一种新的方法。 The condensation of hydrazide with benzylideneacetophenone was studied by using phospho-tungstic acid as catalyst. After a series of reaction conditions, the optimal reaction conditions were established, and the universality of the substrate was investigated. A series of acylhydrazones were obtained with the high yields, up to 99%. The reaction was simple and mild, which provided a new method for the synthesis of chalcone hydrazone.","PeriodicalId":16596,"journal":{"name":"Journal of Organic Chemistry Research","volume":"8 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2016-12-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82181715","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2016-12-02DOI: 10.12677/JOCR.2016.44014
陈向莹, 范芳芳, 夏佳美, 张千峰
以2,3,5-三甲基吡啶为起始原料，经N-氧化、硝化、亲核取代、重排水解和氯甲基化等五大步骤而制得2-氯甲基-3,5-二甲基-4-甲氧基吡啶的合成与工艺。并通过1HNMR、FT-IR、HPLC等测试手段对2-氯甲基-3,5-二甲基-4-甲氧基吡啶产品进行定性和定量分析。 2-Chloromethyl-3,5-dimethyl-4-methoxypyridine was synthesized by use of 2,3,5-trimethylpyridine as the starting material. The synthetic route contains five steps including N-oxidation, nitration, nu-cleophilic substitution, alcoholation and chloromethylation. The target product was qualitatively and quantitatively analyzed using 1H NMR, FT-IR, and HPLC testing methods.
以2,3,5-三甲基吡啶为起始原料，经N-氧化、硝化、亲核取代、重排水解和氯甲基化等五大步骤而制得2-氯甲基-3,5-二甲基-4-甲氧基吡啶的合成与工艺。并通过1HNMR、FT-IR、HPLC等测试手段对2-氯甲基-3,5-二甲基-4-甲氧基吡啶产品进行定性和定量分析。 2-Chloromethyl-3,5-dimethyl-4-methoxypyridine was synthesized by use of 2,3,5-trimethylpyridine as the starting material. The synthetic route contains five steps including N-oxidation, nitration, nu-cleophilic substitution, alcoholation and chloromethylation. The target product was qualitatively and quantitatively analyzed using 1H NMR, FT-IR, and HPLC testing methods.
{"title":"2-氯甲基-3,5-二甲基-4-甲氧基吡啶的合成及分析 Synthesis and Analysis of 2-Chloromethyl-3,5-Dimethyl-4-Methoxypyridine","authors":"陈向莹, 范芳芳, 夏佳美, 张千峰","doi":"10.12677/JOCR.2016.44014","DOIUrl":"https://doi.org/10.12677/JOCR.2016.44014","url":null,"abstract":"以2,3,5-三甲基吡啶为起始原料，经N-氧化、硝化、亲核取代、重排水解和氯甲基化等五大步骤而制得2-氯甲基-3,5-二甲基-4-甲氧基吡啶的合成与工艺。并通过1HNMR、FT-IR、HPLC等测试手段对2-氯甲基-3,5-二甲基-4-甲氧基吡啶产品进行定性和定量分析。 2-Chloromethyl-3,5-dimethyl-4-methoxypyridine was synthesized by use of 2,3,5-trimethylpyridine as the starting material. The synthetic route contains five steps including N-oxidation, nitration, nu-cleophilic substitution, alcoholation and chloromethylation. The target product was qualitatively and quantitatively analyzed using 1H NMR, FT-IR, and HPLC testing methods.","PeriodicalId":16596,"journal":{"name":"Journal of Organic Chemistry Research","volume":"48 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2016-12-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90745116","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2016-09-09DOI: 10.12677/JOCR.2016.43012
粉玲 李
以番薯叶为原料，采用超声波辅助提取精制多糖，通过高岭土、活性炭、过氧化氢设置各个量进行脱色反应，以及采用分光光度法测定脱色后的吸光度，计算脱色率。研究结果表明番薯叶在高岭土、活性炭、过氧化氢溶液中，在适宜条件下均有较好的脱色效果，其中，活性炭的脱色效果最好。 With sweet potato leaves as raw material, the ultrasonic assisted extraction has been used to refine polysaccharide through setting the kaolin clay, activated carbon and hydrogen peroxide amount to carry on the decolorizing reaction, using spectrophotometry after decolorizing absorbance, and decoloring rate calculation. Some research results show that the sweet potato leaves have good decolorization effect in kaolin clay, activated carbon, hydrogen peroxide solution, under appropriate conditions.
以番薯叶为原料，采用超声波辅助提取精制多糖，通过高岭土、活性炭、过氧化氢设置各个量进行脱色反应，以及采用分光光度法测定脱色后的吸光度，计算脱色率。研究结果表明番薯叶在高岭土、活性炭、过氧化氢溶液中，在适宜条件下均有较好的脱色效果，其中，活性炭的脱色效果最好。 With sweet potato leaves as raw material, the ultrasonic assisted extraction has been used to refine polysaccharide through setting the kaolin clay, activated carbon and hydrogen peroxide amount to carry on the decolorizing reaction, using spectrophotometry after decolorizing absorbance, and decoloring rate calculation. Some research results show that the sweet potato leaves have good decolorization effect in kaolin clay, activated carbon, hydrogen peroxide solution, under appropriate conditions.
{"title":"Decoloring Research on Sweet Potato Leaf","authors":"粉玲 李","doi":"10.12677/JOCR.2016.43012","DOIUrl":"https://doi.org/10.12677/JOCR.2016.43012","url":null,"abstract":"以番薯叶为原料，采用超声波辅助提取精制多糖，通过高岭土、活性炭、过氧化氢设置各个量进行脱色反应，以及采用分光光度法测定脱色后的吸光度，计算脱色率。研究结果表明番薯叶在高岭土、活性炭、过氧化氢溶液中，在适宜条件下均有较好的脱色效果，其中，活性炭的脱色效果最好。 With sweet potato leaves as raw material, the ultrasonic assisted extraction has been used to refine polysaccharide through setting the kaolin clay, activated carbon and hydrogen peroxide amount to carry on the decolorizing reaction, using spectrophotometry after decolorizing absorbance, and decoloring rate calculation. Some research results show that the sweet potato leaves have good decolorization effect in kaolin clay, activated carbon, hydrogen peroxide solution, under appropriate conditions.","PeriodicalId":16596,"journal":{"name":"Journal of Organic Chemistry Research","volume":"8 1","pages":"82-92"},"PeriodicalIF":0.0,"publicationDate":"2016-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78316837","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2016-09-09DOI: 10.12677/JOCR.2016.43011
李 伟杰
在缩合剂N,N'-二环己基碳二亚胺(DCC)和催化剂4-二甲氨基吡啶(DMAP)的作用下，羽扇烷醇与过量的没食子酸在二氯甲烷中回流10 h，合成了新化合物没食子酸羽扇烷醇酯，产率为69.6%。研究了没食子酸羽扇烷醇酯体外对肿瘤细胞株A549、LAC和HepG2的抑制活性。结果表明，羽扇烷醇和顺铂作为阳性对照物，它们对上述3株肿瘤细胞株的增殖没有抑制作用，没食子酸羽扇烷醇酯对A549、LAC和HepG2的IC50值分别是51.71、62.16和64.34 μM，其对肿瘤细胞株A549和LAC增殖的抑制作用不及阿霉素，而对HepG2增殖的抑制作用比阿霉素的强。 Under the presence of N,N'-dicyclohexylcarbodiimide (DDC) as dehydrating agent and 4-dimethyl- aminopyridine (DMAP) as catalyst, lupanol was refluxed with excessive gallic acid for 10 h in di-chloromethane to give lupanol gallate as a new compound at 69.6% yield. The latter was explored for in vitro antitumor activities against A549, LAC and HepG2 cell lines. The results showed that lupanol and cisplatin as positive control compounds had no inhibitory abilities against the above three tested tumor cell lines. The IC50 values of lupanol gallate against A549, LAC and HepG2 cells were 51.71 μM, 62.16 μM and 64.34 μM respectively. The antitumor activities of lupanol gallate against A549 and LAC cells were inferior to those of adriamycin, however its antitumor activity against HepG2 cell exceeded that of adriamycin.
在缩合剂N,N'-二环己基碳二亚胺(DCC)和催化剂4-二甲氨基吡啶(DMAP)的作用下，羽扇烷醇与过量的没食子酸在二氯甲烷中回流10 h，合成了新化合物没食子酸羽扇烷醇酯，产率为69.6%。研究了没食子酸羽扇烷醇酯体外对肿瘤细胞株A549、LAC和HepG2的抑制活性。结果表明，羽扇烷醇和顺铂作为阳性对照物，它们对上述3株肿瘤细胞株的增殖没有抑制作用，没食子酸羽扇烷醇酯对A549、LAC和HepG2的IC50值分别是51.71、62.16和64.34 μM，其对肿瘤细胞株A549和LAC增殖的抑制作用不及阿霉素，而对HepG2增殖的抑制作用比阿霉素的强。 Under the presence of N,N'-dicyclohexylcarbodiimide (DDC) as dehydrating agent and 4-dimethyl- aminopyridine (DMAP) as catalyst, lupanol was refluxed with excessive gallic acid for 10 h in di-chloromethane to give lupanol gallate as a new compound at 69.6% yield. The latter was explored for in vitro antitumor activities against A549, LAC and HepG2 cell lines. The results showed that lupanol and cisplatin as positive control compounds had no inhibitory abilities against the above three tested tumor cell lines. The IC50 values of lupanol gallate against A549, LAC and HepG2 cells were 51.71 μM, 62.16 μM and 64.34 μM respectively. The antitumor activities of lupanol gallate against A549 and LAC cells were inferior to those of adriamycin, however its antitumor activity against HepG2 cell exceeded that of adriamycin.
{"title":"Synthesis and In Vitro Antitumor Activities of Lupanol Gallate","authors":"李 伟杰","doi":"10.12677/JOCR.2016.43011","DOIUrl":"https://doi.org/10.12677/JOCR.2016.43011","url":null,"abstract":"在缩合剂N,N'-二环己基碳二亚胺(DCC)和催化剂4-二甲氨基吡啶(DMAP)的作用下，羽扇烷醇与过量的没食子酸在二氯甲烷中回流10 h，合成了新化合物没食子酸羽扇烷醇酯，产率为69.6%。研究了没食子酸羽扇烷醇酯体外对肿瘤细胞株A549、LAC和HepG2的抑制活性。结果表明，羽扇烷醇和顺铂作为阳性对照物，它们对上述3株肿瘤细胞株的增殖没有抑制作用，没食子酸羽扇烷醇酯对A549、LAC和HepG2的IC50值分别是51.71、62.16和64.34 μM，其对肿瘤细胞株A549和LAC增殖的抑制作用不及阿霉素，而对HepG2增殖的抑制作用比阿霉素的强。 Under the presence of N,N'-dicyclohexylcarbodiimide (DDC) as dehydrating agent and 4-dimethyl- aminopyridine (DMAP) as catalyst, lupanol was refluxed with excessive gallic acid for 10 h in di-chloromethane to give lupanol gallate as a new compound at 69.6% yield. The latter was explored for in vitro antitumor activities against A549, LAC and HepG2 cell lines. The results showed that lupanol and cisplatin as positive control compounds had no inhibitory abilities against the above three tested tumor cell lines. The IC50 values of lupanol gallate against A549, LAC and HepG2 cells were 51.71 μM, 62.16 μM and 64.34 μM respectively. The antitumor activities of lupanol gallate against A549 and LAC cells were inferior to those of adriamycin, however its antitumor activity against HepG2 cell exceeded that of adriamycin.","PeriodicalId":16596,"journal":{"name":"Journal of Organic Chemistry Research","volume":"19 1","pages":"77-81"},"PeriodicalIF":0.0,"publicationDate":"2016-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75641739","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2016-09-09DOI: 10.12677/JOCR.2016.43010
吴 静姝
在综述秃马勃属真菌化学成分研究的基础上，通过多种指示剂和显色剂的显色反应或沉淀反应对佛山白秃马勃化学成分进行了预分析，并通过羟自由基(•OH)和1,1-二苯基-2-苦肼基(DPPH)清除试验评价了其甲醇提取物的体外抗氧化活性。结果表明，佛山白秃马勃含有生物碱、甾体和萜类化合物，具有有效的抗氧化活性，对•OH和DPPH自由基的半数清除浓度(IC50)分别为241.55和418.63 μg/mL。 Based on review of chemical composition of the genus of Calvatia sp., the chemical constituents of the puffball Calvatia candida from Foshan were analyzed by pre-test tube method, and its antioxi-dant activities were evaluated by the biochemical assay of hydroxyl and DPPH radicals scavenging activity in vitro. The results show that, the puffball Calvatia candida from Foshan contain alkaloids, steroids and terpenoids, and have potent antioxidant activities with IC50 values of 241.55 (for •OH) and 418.63 (for DPPH) μg/mL, respectively.
在综述秃马勃属真菌化学成分研究的基础上，通过多种指示剂和显色剂的显色反应或沉淀反应对佛山白秃马勃化学成分进行了预分析，并通过羟自由基(•OH)和1,1-二苯基-2-苦肼基(DPPH)清除试验评价了其甲醇提取物的体外抗氧化活性。结果表明，佛山白秃马勃含有生物碱、甾体和萜类化合物，具有有效的抗氧化活性，对•OH和DPPH自由基的半数清除浓度(IC50)分别为241.55和418.63 μg/mL。 Based on review of chemical composition of the genus of Calvatia sp., the chemical constituents of the puffball Calvatia candida from Foshan were analyzed by pre-test tube method, and its antioxi-dant activities were evaluated by the biochemical assay of hydroxyl and DPPH radicals scavenging activity in vitro. The results show that, the puffball Calvatia candida from Foshan contain alkaloids, steroids and terpenoids, and have potent antioxidant activities with IC50 values of 241.55 (for •OH) and 418.63 (for DPPH) μg/mL, respectively.
{"title":"Chemical Constituents Pre-Analysis and Antioxidant Activity of the Puffball Calvatia candida from Foshan","authors":"吴 静姝","doi":"10.12677/JOCR.2016.43010","DOIUrl":"https://doi.org/10.12677/JOCR.2016.43010","url":null,"abstract":"在综述秃马勃属真菌化学成分研究的基础上，通过多种指示剂和显色剂的显色反应或沉淀反应对佛山白秃马勃化学成分进行了预分析，并通过羟自由基(•OH)和1,1-二苯基-2-苦肼基(DPPH)清除试验评价了其甲醇提取物的体外抗氧化活性。结果表明，佛山白秃马勃含有生物碱、甾体和萜类化合物，具有有效的抗氧化活性，对•OH和DPPH自由基的半数清除浓度(IC50)分别为241.55和418.63 μg/mL。 Based on review of chemical composition of the genus of Calvatia sp., the chemical constituents of the puffball Calvatia candida from Foshan were analyzed by pre-test tube method, and its antioxi-dant activities were evaluated by the biochemical assay of hydroxyl and DPPH radicals scavenging activity in vitro. The results show that, the puffball Calvatia candida from Foshan contain alkaloids, steroids and terpenoids, and have potent antioxidant activities with IC50 values of 241.55 (for •OH) and 418.63 (for DPPH) μg/mL, respectively.","PeriodicalId":16596,"journal":{"name":"Journal of Organic Chemistry Research","volume":"22 1","pages":"69-76"},"PeriodicalIF":0.0,"publicationDate":"2016-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75302322","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2016-09-09DOI: 10.12677/JOCR.2016.43009
于治梅, 廖兴龙, 蔚建勇, 杨大成
芳香醛、芳香酮和芳香胺参与的Mannich反应，其合成方法和甲醛参与的Mannich反应差别较大，生成的某些Mannich碱显示多方面的生物活性，包括抗糖尿病、抗肿瘤、抗微生物和抗结核等活性。本文主要总结和讨论此类Mannich反应的发展历程及曼尼碱的生物活性，希望对相关研究人员有一定的参考价值。 The Mannich reaction of aromatic aldehydes, aromatic ketones with aromatic amines has re-markable difference in synthetic method compared with that of Mannich reaction of formaldehyde. Some Mannich bases exhibit specific biological activity, such as antidiabetic, antimicrobial, anti-tumor, and anti-tuberculosis activity. This paper primarily summarizes the development history of this kind of Mannich reaction and further introduces their biological activities mainly discovered by our lab, and hope to provide hint for future investigation of this Mannich reaction.
芳香醛、芳香酮和芳香胺参与的Mannich反应，其合成方法和甲醛参与的Mannich反应差别较大，生成的某些Mannich碱显示多方面的生物活性，包括抗糖尿病、抗肿瘤、抗微生物和抗结核等活性。本文主要总结和讨论此类Mannich反应的发展历程及曼尼碱的生物活性，希望对相关研究人员有一定的参考价值。 The Mannich reaction of aromatic aldehydes, aromatic ketones with aromatic amines has re-markable difference in synthetic method compared with that of Mannich reaction of formaldehyde. Some Mannich bases exhibit specific biological activity, such as antidiabetic, antimicrobial, anti-tumor, and anti-tuberculosis activity. This paper primarily summarizes the development history of this kind of Mannich reaction and further introduces their biological activities mainly discovered by our lab, and hope to provide hint for future investigation of this Mannich reaction.
{"title":"芳香醛、芳香酮和芳香胺的Mannich反应研究概况 Advances in the Mannich Reaction of Aromatic Aldehydes, Aromatic Ketones with Aromatic Amines","authors":"于治梅, 廖兴龙, 蔚建勇, 杨大成","doi":"10.12677/JOCR.2016.43009","DOIUrl":"https://doi.org/10.12677/JOCR.2016.43009","url":null,"abstract":"芳香醛、芳香酮和芳香胺参与的Mannich反应，其合成方法和甲醛参与的Mannich反应差别较大，生成的某些Mannich碱显示多方面的生物活性，包括抗糖尿病、抗肿瘤、抗微生物和抗结核等活性。本文主要总结和讨论此类Mannich反应的发展历程及曼尼碱的生物活性，希望对相关研究人员有一定的参考价值。 The Mannich reaction of aromatic aldehydes, aromatic ketones with aromatic amines has re-markable difference in synthetic method compared with that of Mannich reaction of formaldehyde. Some Mannich bases exhibit specific biological activity, such as antidiabetic, antimicrobial, anti-tumor, and anti-tuberculosis activity. This paper primarily summarizes the development history of this kind of Mannich reaction and further introduces their biological activities mainly discovered by our lab, and hope to provide hint for future investigation of this Mannich reaction.","PeriodicalId":16596,"journal":{"name":"Journal of Organic Chemistry Research","volume":"3 1","pages":"61-68"},"PeriodicalIF":0.0,"publicationDate":"2016-09-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82628943","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2016-06-07DOI: 10.12677/JOCR.2016.42007
阿地里江 bull, 吾买尔江, 李文博, 夏米西努尔 bull, 艾力
本文报道了在离子液体[Bmim]BF4催化下以丙酰乙酸甲酯或丙酰乙酸乙酯，苯肼，芳醛和丙二腈等四组分为原料经过一锅法合成了一系列多取代吡喃[2,3-c]吡唑类化合物的方法。该方法具有方便，产率较高等特点，为合成此类化合物提供了一个参考依据。产物的结构通过IR，1H NMR和MS进行表征。 A series of multi-substituted pyrano[2,3-c]pyrazole derivatives were synthesized by one-pot reac-tion of ethyl propionyl acetate, phenylhydrazine, aromatic aldehyde and malononitrile. We developed an efficient and convenient method for the synthesis of multi-substituted pyrano[2,3-c]pyrazoles in high yields using ionic liquid [Bmim]BF4 as a catalyst. And structures of the products were characterized by IR, 1H NMR and MS.
本文报道了在离子液体[Bmim]BF4催化下以丙酰乙酸甲酯或丙酰乙酸乙酯，苯肼，芳醛和丙二腈等四组分为原料经过一锅法合成了一系列多取代吡喃[2,3-c]吡唑类化合物的方法。该方法具有方便，产率较高等特点，为合成此类化合物提供了一个参考依据。产物的结构通过IR，1H NMR和MS进行表征。 A series of multi-substituted pyrano[2,3-c]pyrazole derivatives were synthesized by one-pot reac-tion of ethyl propionyl acetate, phenylhydrazine, aromatic aldehyde and malononitrile. We developed an efficient and convenient method for the synthesis of multi-substituted pyrano[2,3-c]pyrazoles in high yields using ionic liquid [Bmim]BF4 as a catalyst. And structures of the products were characterized by IR, 1H NMR and MS.
{"title":"多取代吡喃[2,3-c]吡唑类化合物的在离子液体[Bmim]BF4催化下的四组分一锅法合成","authors":"阿地里江 bull, 吾买尔江, 李文博, 夏米西努尔 bull, 艾力","doi":"10.12677/JOCR.2016.42007","DOIUrl":"https://doi.org/10.12677/JOCR.2016.42007","url":null,"abstract":"本文报道了在离子液体[Bmim]BF4催化下以丙酰乙酸甲酯或丙酰乙酸乙酯，苯肼，芳醛和丙二腈等四组分为原料经过一锅法合成了一系列多取代吡喃[2,3-c]吡唑类化合物的方法。该方法具有方便，产率较高等特点，为合成此类化合物提供了一个参考依据。产物的结构通过IR，1H NMR和MS进行表征。 A series of multi-substituted pyrano[2,3-c]pyrazole derivatives were synthesized by one-pot reac-tion of ethyl propionyl acetate, phenylhydrazine, aromatic aldehyde and malononitrile. We developed an efficient and convenient method for the synthesis of multi-substituted pyrano[2,3-c]pyrazoles in high yields using ionic liquid [Bmim]BF4 as a catalyst. And structures of the products were characterized by IR, 1H NMR and MS.","PeriodicalId":16596,"journal":{"name":"Journal of Organic Chemistry Research","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2016-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74548240","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2016-06-07DOI: 10.12677/JOCR.2016.42004
Xiaoli Sun, Li Fan, Xue-mei Tang, Dacheng Yang
氯化亚砜是由醇制备氯代烃、羧酸制备酰氯的常用试剂，在精细化工产品和有机化工中间体的合成中具有广泛的应用。但是氯化亚砜-醇体系的应用在文献中报道并不多。本文主要综述氯化亚砜-醇体系在羧酸酯化、酰胺脱酰化、羧酸酯化和酰胺脱酰化双重作用等的研究进展。 Thionyl chloride (SOCl2) is a common reagent for the preparation of chlorinated hydrocarbons originated from alcohols and acyl chloride from carboxylic acids. Although SOCl2 is widely used in the synthesis of fine chemicals and pharmaceutical intermediates, the report about the application of thionyl chloride-alcohol system (SOCl2/ROH) is not too much. In this paper, the research progresses on SOCl2/ROH in esterification of carboxylic acid, deacylation of amide, and the dual role of esterification and deacylation are reviewed comprehensively.
氯化亚砜是由醇制备氯代烃、羧酸制备酰氯的常用试剂，在精细化工产品和有机化工中间体的合成中具有广泛的应用。但是氯化亚砜-醇体系的应用在文献中报道并不多。本文主要综述氯化亚砜-醇体系在羧酸酯化、酰胺脱酰化、羧酸酯化和酰胺脱酰化双重作用等的研究进展。 Thionyl chloride (SOCl2) is a common reagent for the preparation of chlorinated hydrocarbons originated from alcohols and acyl chloride from carboxylic acids. Although SOCl2 is widely used in the synthesis of fine chemicals and pharmaceutical intermediates, the report about the application of thionyl chloride-alcohol system (SOCl2/ROH) is not too much. In this paper, the research progresses on SOCl2/ROH in esterification of carboxylic acid, deacylation of amide, and the dual role of esterification and deacylation are reviewed comprehensively.
{"title":"Application of Thionyl Chloride-Alcohol System in Organic Synthesis","authors":"Xiaoli Sun, Li Fan, Xue-mei Tang, Dacheng Yang","doi":"10.12677/JOCR.2016.42004","DOIUrl":"https://doi.org/10.12677/JOCR.2016.42004","url":null,"abstract":"氯化亚砜是由醇制备氯代烃、羧酸制备酰氯的常用试剂，在精细化工产品和有机化工中间体的合成中具有广泛的应用。但是氯化亚砜-醇体系的应用在文献中报道并不多。本文主要综述氯化亚砜-醇体系在羧酸酯化、酰胺脱酰化、羧酸酯化和酰胺脱酰化双重作用等的研究进展。 Thionyl chloride (SOCl2) is a common reagent for the preparation of chlorinated hydrocarbons originated from alcohols and acyl chloride from carboxylic acids. Although SOCl2 is widely used in the synthesis of fine chemicals and pharmaceutical intermediates, the report about the application of thionyl chloride-alcohol system (SOCl2/ROH) is not too much. In this paper, the research progresses on SOCl2/ROH in esterification of carboxylic acid, deacylation of amide, and the dual role of esterification and deacylation are reviewed comprehensively.","PeriodicalId":16596,"journal":{"name":"Journal of Organic Chemistry Research","volume":"15 1","pages":"23-32"},"PeriodicalIF":0.0,"publicationDate":"2016-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87784744","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2016-06-07DOI: 10.12677/JOCR.2016.42008
麦麦提艾力 bull, 奥布力, 再乃普古丽 bull, 伊斯马伊力, 马夏冰
本文主要介绍了合成一系列N-(4-芳基噻唑-2-基)-对苄氧基苯乙酮腙类化合物的简单方法，这些化合物已得到1HNMR和IR光谱确证。该方法具有操作简便，经济和环保等优点。 This paper mainly described the synthesis of hydrazone derivatives of N-(4-aryl-thiazol-2-yl)- benzyloxy-acetophenone. All compounds were confirmed by 1HNMR and IR spectrography. This method can operate simply and is economical and environment-friendly.
本文主要介绍了合成一系列N-(4-芳基噻唑-2-基)-对苄氧基苯乙酮腙类化合物的简单方法，这些化合物已得到1HNMR和IR光谱确证。该方法具有操作简便，经济和环保等优点。 This paper mainly described the synthesis of hydrazone derivatives of N-(4-aryl-thiazol-2-yl)- benzyloxy-acetophenone. All compounds were confirmed by 1HNMR and IR spectrography. This method can operate simply and is economical and environment-friendly.
{"title":"N-(4-芳基噻唑-2-基)-对苄氧基苯乙酮腙的合成","authors":"麦麦提艾力 bull, 奥布力, 再乃普古丽 bull, 伊斯马伊力, 马夏冰","doi":"10.12677/JOCR.2016.42008","DOIUrl":"https://doi.org/10.12677/JOCR.2016.42008","url":null,"abstract":"本文主要介绍了合成一系列N-(4-芳基噻唑-2-基)-对苄氧基苯乙酮腙类化合物的简单方法，这些化合物已得到1HNMR和IR光谱确证。该方法具有操作简便，经济和环保等优点。 This paper mainly described the synthesis of hydrazone derivatives of N-(4-aryl-thiazol-2-yl)- benzyloxy-acetophenone. All compounds were confirmed by 1HNMR and IR spectrography. This method can operate simply and is economical and environment-friendly.","PeriodicalId":16596,"journal":{"name":"Journal of Organic Chemistry Research","volume":"22 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2016-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73875694","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2016-06-07DOI: 10.12677/JOCR.2016.42006
刘威威, 姜伟伟, 唐维克, 冯乙巳
本研究采用浸渍法制作了一系列的以γ-Al2O3为载体的Pd-Ni双金属纳米催化剂(Pd-Ni(x: y)/Al2O3；x和y分别是Pd-Ni的摩尔比)，该催化剂用于二甲基丙二胺和二甲氨基丙腈加氢合成四甲基二丙烯三胺。并使用X射线衍射(XRD)、X电子光谱法(XPS)和透射电子显微镜法(TEM)对催化剂进行了表征。催化剂的活性随着Pd-Ni负载量的不同而变化。在所有催化剂中Pd-Ni/γ-Al2O3 (Pd:Ni = 1:2)表现出了最佳的催化活性，转化率在30%~40%，选择性达到90% (120˚C, 最初氢气压力2 MPa, 8 h)。 Several γ-Al2O3 supported Pd-Ni bimetallic nanocatalysts (Pd-Ni(x:y)/Al2O3; where x and y repre-sent the mass ratio of Pd and Ni, respectively) were prepared by the impregnation method and used for selective hydrogenation of N,N-Dimethyl-1,3-propane diamine and Dimethylaminopropionitrile to 3,3’-iminobis(N,N-dimethylpropylamine). The Pd-Ni/Al2O3 samples were confirmed to have generated Pd-Ni bimetallic nanoparticles by X-ray diffraction (XRD), X-ray photoelectron spec-troscopy (XPS) and transmission electron microscopy (TEM). The catalytic activity was assessed in view of the effects of different mass ratios of Pd and Ni. Among all the samples, the Pd-Ni (1:2)/Al2O3 (PN-1:1) catalyst showed extremely high catalytic ability, which had 30% - 40% conversion rate and 90% selectivity (120˚C, 2 MPa initial H2 pressure, 8 h).
本研究采用浸渍法制作了一系列的以γ-Al2O3为载体的Pd-Ni双金属纳米催化剂(Pd-Ni(x: y)/Al2O3；x和y分别是Pd-Ni的摩尔比)，该催化剂用于二甲基丙二胺和二甲氨基丙腈加氢合成四甲基二丙烯三胺。并使用X射线衍射(XRD)、X电子光谱法(XPS)和透射电子显微镜法(TEM)对催化剂进行了表征。催化剂的活性随着Pd-Ni负载量的不同而变化。在所有催化剂中Pd-Ni/γ-Al2O3 (Pd:Ni = 1:2)表现出了最佳的催化活性，转化率在30%~40%，选择性达到90% (120˚C, 最初氢气压力2 MPa, 8 h)。 Several γ-Al2O3 supported Pd-Ni bimetallic nanocatalysts (Pd-Ni(x:y)/Al2O3; where x and y repre-sent the mass ratio of Pd and Ni, respectively) were prepared by the impregnation method and used for selective hydrogenation of N,N-Dimethyl-1,3-propane diamine and Dimethylaminopropionitrile to 3,3’-iminobis(N,N-dimethylpropylamine). The Pd-Ni/Al2O3 samples were confirmed to have generated Pd-Ni bimetallic nanoparticles by X-ray diffraction (XRD), X-ray photoelectron spec-troscopy (XPS) and transmission electron microscopy (TEM). The catalytic activity was assessed in view of the effects of different mass ratios of Pd and Ni. Among all the samples, the Pd-Ni (1:2)/Al2O3 (PN-1:1) catalyst showed extremely high catalytic ability, which had 30% - 40% conversion rate and 90% selectivity (120˚C, 2 MPa initial H2 pressure, 8 h).
{"title":"Pd-Ni/Al2O3催化合成四甲基二丙烯三胺研究 Pd-Ni/Al2O3 Catalyze Synthesis of 3,3’-Iminobis(N,N-dimethylpropylamine)","authors":"刘威威, 姜伟伟, 唐维克, 冯乙巳","doi":"10.12677/JOCR.2016.42006","DOIUrl":"https://doi.org/10.12677/JOCR.2016.42006","url":null,"abstract":"本研究采用浸渍法制作了一系列的以γ-Al2O3为载体的Pd-Ni双金属纳米催化剂(Pd-Ni(x: y)/Al2O3；x和y分别是Pd-Ni的摩尔比)，该催化剂用于二甲基丙二胺和二甲氨基丙腈加氢合成四甲基二丙烯三胺。并使用X射线衍射(XRD)、X电子光谱法(XPS)和透射电子显微镜法(TEM)对催化剂进行了表征。催化剂的活性随着Pd-Ni负载量的不同而变化。在所有催化剂中Pd-Ni/γ-Al2O3 (Pd:Ni = 1:2)表现出了最佳的催化活性，转化率在30%~40%，选择性达到90% (120˚C, 最初氢气压力2 MPa, 8 h)。 Several γ-Al2O3 supported Pd-Ni bimetallic nanocatalysts (Pd-Ni(x:y)/Al2O3; where x and y repre-sent the mass ratio of Pd and Ni, respectively) were prepared by the impregnation method and used for selective hydrogenation of N,N-Dimethyl-1,3-propane diamine and Dimethylaminopropionitrile to 3,3’-iminobis(N,N-dimethylpropylamine). The Pd-Ni/Al2O3 samples were confirmed to have generated Pd-Ni bimetallic nanoparticles by X-ray diffraction (XRD), X-ray photoelectron spec-troscopy (XPS) and transmission electron microscopy (TEM). The catalytic activity was assessed in view of the effects of different mass ratios of Pd and Ni. Among all the samples, the Pd-Ni (1:2)/Al2O3 (PN-1:1) catalyst showed extremely high catalytic ability, which had 30% - 40% conversion rate and 90% selectivity (120˚C, 2 MPa initial H2 pressure, 8 h).","PeriodicalId":16596,"journal":{"name":"Journal of Organic Chemistry Research","volume":"3 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2016-06-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88482973","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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