The compound 1-(3-chlorophenyl)-3-(6-((1,7,7-trimethylbicyclo[2.2.1]heptan-2-ylidene)amino)hexyl)thiourea was synthesized for the first time from 6-((1,7,7-trimethylbicyclo[2.2.1]heptan-2-ylidene)amino)hexan-1-amine and 3-chlorophenylisothiocyanate in DMF with a 60% yield. It was characterized by 1H, 13C{1H} NMR, FT-IR, MS, and elemental analysis.
{"title":"1-(3-Chlorophenyl)-3-(6-((1,7,7-trimethylbicyclo[2.2.1]heptan-2-ylidene)amino)hexyl)thiourea","authors":"Daria Zapravdina, V. Burmistrov","doi":"10.3390/m1809","DOIUrl":"https://doi.org/10.3390/m1809","url":null,"abstract":"The compound 1-(3-chlorophenyl)-3-(6-((1,7,7-trimethylbicyclo[2.2.1]heptan-2-ylidene)amino)hexyl)thiourea was synthesized for the first time from 6-((1,7,7-trimethylbicyclo[2.2.1]heptan-2-ylidene)amino)hexan-1-amine and 3-chlorophenylisothiocyanate in DMF with a 60% yield. It was characterized by 1H, 13C{1H} NMR, FT-IR, MS, and elemental analysis.","PeriodicalId":509184,"journal":{"name":"Molbank","volume":" 5","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-04-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140685845","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}
The one-pot template reaction between 2-(diphenylphosphino)benzaldehyde, benzylamine and copper(I) iodide yields the dinuclear copper complex (P∩N)2Cu2I2, as revealed by single-crystal X-ray diffraction.
单晶 X 射线衍射显示，2-(二苯基膦)苯甲醛、苄胺和碘化铜（I）之间的单锅模板反应生成了双核铜络合物 (P∩N)2Cu2I2。
{"title":"Diiodido-bis{N-[2-(diphenylphosphino)benzylidene]benzylamine-κ2N,P}dicopper(I)","authors":"J. Süß, Uwe Monkowius, M. Zabel","doi":"10.3390/m1808","DOIUrl":"https://doi.org/10.3390/m1808","url":null,"abstract":"The one-pot template reaction between 2-(diphenylphosphino)benzaldehyde, benzylamine and copper(I) iodide yields the dinuclear copper complex (P∩N)2Cu2I2, as revealed by single-crystal X-ray diffraction.","PeriodicalId":509184,"journal":{"name":"Molbank","volume":" 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-04-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140686184","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}
M. Mori, Giulia Cazzaniga, Donatella Nava, Elena Pini
In the context of our ongoing studies on chromane derivatives as inhibitors of the salicylate synthase from M. tuberculosis, we isolated a new, unexpected compound from the cyclization of 3-(propargyloxy)-5-benzyloxy-benzoic acid methyl ester. Its molecular structure was elucidated by means of 1D and 2D NMR analyses, FT-IR, ESI-MS, and HRMS.
{"title":"Synthesis and Analytical Characterization of Cyclization Products of 3-Propargyloxy-5-benzyloxy-benzoic Acid Methyl Ester","authors":"M. Mori, Giulia Cazzaniga, Donatella Nava, Elena Pini","doi":"10.3390/m1806","DOIUrl":"https://doi.org/10.3390/m1806","url":null,"abstract":"In the context of our ongoing studies on chromane derivatives as inhibitors of the salicylate synthase from M. tuberculosis, we isolated a new, unexpected compound from the cyclization of 3-(propargyloxy)-5-benzyloxy-benzoic acid methyl ester. Its molecular structure was elucidated by means of 1D and 2D NMR analyses, FT-IR, ESI-MS, and HRMS.","PeriodicalId":509184,"journal":{"name":"Molbank","volume":"2 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-04-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140696950","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}
The reaction of the potassium salt of (2,6-diisopropylphenyl)-[6-(2,4,6-triisopropylphenyl)-pyridine-2-yl]-amine (Ap*H) with the equimolar ratio of [ScCl3] in tetrahydrofuran (thf) resulted in the mononuclear mono(aminopyridinato) scandium dichloride complex [Ap*ScCl2(thf)2]. An X-ray analysis showed the title compound to be monomeric. The compound [C40H59Cl2N2O2Sc] crystallized in the monoclinic space group, P21/n, and possessed the following cell parameters: a = 12.4441(8) b = 22.9975(10) c = 13.9971(8) Å, β = 92.297(5)°, V = 4002.5(4) A3, and Z = 4. Hirshfeld analyses show that H…H (91.1%), H…C/C…H (5.0%), and H…Cl/Cl…H (3.9%) are the contributing interactions in the solid-state structure. The compound was further characterized by NMR spectroscopy, and its purity was confirmed by elemental analysis.
(2,6-二异丙基苯基)-[6-(2,4,6-三异丙基苯基)-吡啶-2-基]-胺（Ap*H）的钾盐与等摩尔比的[ScCl3]在四氢呋喃（thf）中反应生成单核单（氨基吡啶）二氯化钪络合物[Ap*ScCl2(thf)2]。X 射线分析表明标题化合物为单体。化合物[C40H59Cl2N2O2Sc]在单斜空间群 P21/n 中结晶，具有以下晶胞参数：a = 12.4441(8) b = 22.9975(10) c = 13.9971(8) Å，β = 92.297(5)°, V = 4002.5(4) A3，Z = 4。Hirshfeld 分析表明，H...H（91.1%）、H...C/C...H（5.0%）和 H...Cl/Cl...H （3.9%）是固态结构中的主要相互作用。通过核磁共振光谱对该化合物进行了进一步表征，并通过元素分析确认了其纯度。
{"title":"The Synthesis and Structure of Scandium Dichloride of Sterically Demanding Aminopyridinato Ligands","authors":"Sadaf Qayyum","doi":"10.3390/m1805","DOIUrl":"https://doi.org/10.3390/m1805","url":null,"abstract":"The reaction of the potassium salt of (2,6-diisopropylphenyl)-[6-(2,4,6-triisopropylphenyl)-pyridine-2-yl]-amine (Ap*H) with the equimolar ratio of [ScCl3] in tetrahydrofuran (thf) resulted in the mononuclear mono(aminopyridinato) scandium dichloride complex [Ap*ScCl2(thf)2]. An X-ray analysis showed the title compound to be monomeric. The compound [C40H59Cl2N2O2Sc] crystallized in the monoclinic space group, P21/n, and possessed the following cell parameters: a = 12.4441(8) b = 22.9975(10) c = 13.9971(8) Å, β = 92.297(5)°, V = 4002.5(4) A3, and Z = 4. Hirshfeld analyses show that H…H (91.1%), H…C/C…H (5.0%), and H…Cl/Cl…H (3.9%) are the contributing interactions in the solid-state structure. The compound was further characterized by NMR spectroscopy, and its purity was confirmed by elemental analysis.","PeriodicalId":509184,"journal":{"name":"Molbank","volume":"26 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-04-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140718122","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}
When 1-benzoylthiosemicarbazide (2) or thiosemicarbazide (1) were treated with benzoyl chloride in a basic medium, a mixture of two compounds was obtained: 1,2-dibenzoylthiosemicarbazide (3) and 1,4-dibenzoylthiosemicarbazide (4). To determine the structure of the novel compounds, 2D NMR spectroscopy techniques such as 1H-13C and 1H-15N were employed.
{"title":"1,2-Dibenzoylthiosemicarbazide","authors":"Burcă Ion, Badea Valentin, Todea Anamaria, Bercean Vasile-Nicolae","doi":"10.3390/m1804","DOIUrl":"https://doi.org/10.3390/m1804","url":null,"abstract":"When 1-benzoylthiosemicarbazide (2) or thiosemicarbazide (1) were treated with benzoyl chloride in a basic medium, a mixture of two compounds was obtained: 1,2-dibenzoylthiosemicarbazide (3) and 1,4-dibenzoylthiosemicarbazide (4). To determine the structure of the novel compounds, 2D NMR spectroscopy techniques such as 1H-13C and 1H-15N were employed.","PeriodicalId":509184,"journal":{"name":"Molbank","volume":"29 2","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-04-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140720968","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}
R. A. Aitken, David B. Cordes, Arun Goyal, Aidan P. McKay
A simplified synthesis of the title compound is reported and its 1H and 13C NMR data are fully assigned including determination of H–H and C–H coupling constants. Its X-ray structure has been determined for the first time. NMR data are also presented for the oxygen analogue.
{"title":"Benzo[d][1,2,3]oxadithiole 2-Oxide","authors":"R. A. Aitken, David B. Cordes, Arun Goyal, Aidan P. McKay","doi":"10.3390/m1803","DOIUrl":"https://doi.org/10.3390/m1803","url":null,"abstract":"A simplified synthesis of the title compound is reported and its 1H and 13C NMR data are fully assigned including determination of H–H and C–H coupling constants. Its X-ray structure has been determined for the first time. NMR data are also presented for the oxygen analogue.","PeriodicalId":509184,"journal":{"name":"Molbank","volume":"8 22","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-04-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140732824","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}
E. Podda, Anna Pintus, V. Lippolis, F. Isaia, Alexandra M. Z. Slawin, C. Carpenter‐Warren, J. Woollins, M. Aragoni
The reactivity of 3,5-di-(pyridin-4-yl)-1,2,4-thiadiazole (L1) with 1,4-diiodotetrafluorobenzene (1,4-DITFB) was explored and the halogen-bonded 1:1 co-crystal (1) was successfully isolated and structurally characterized.
{"title":"1,4-Diiodotetrafluorobenzene 3,5-di-(pyridin-4-yl)-1,2,4-thiadiazole <1/1>","authors":"E. Podda, Anna Pintus, V. Lippolis, F. Isaia, Alexandra M. Z. Slawin, C. Carpenter‐Warren, J. Woollins, M. Aragoni","doi":"10.3390/m1801","DOIUrl":"https://doi.org/10.3390/m1801","url":null,"abstract":"The reactivity of 3,5-di-(pyridin-4-yl)-1,2,4-thiadiazole (L1) with 1,4-diiodotetrafluorobenzene (1,4-DITFB) was explored and the halogen-bonded 1:1 co-crystal (1) was successfully isolated and structurally characterized.","PeriodicalId":509184,"journal":{"name":"Molbank","volume":"62 ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140775054","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}
Guo Yuzhu, Margrate Anyanwu, Xiao Yang, Ren Zimo, Alessandra Gianoncelli, Giovanni Ribaudo, P. Coghi
In this report, we discuss the synthesis of a compound obtained from the derivatization of the natural compound celastrol. This derivative is connected to PEG azide moiety through an amide linkage. The linkage was achieved through the activation of the carboxylic acid using HOBt/EDC. The compound was fully characterized by proton (1H), carbon-13 (13C), heteronuclear single quantum coherence (HSQC), correlation spectroscopy (1H-1H-COSY), and distortionless enhancement by polarization transfer (DEPT) NMR. Ultraviolet (UV), Fourier-transform infrared (FTIR), and high-resolution mass spectrometry (HRMS) were also adopted. Computational investigations were conducted to forecast the binding mode between the synthesized compound and sarco-endoplasmic reticulum (SR) Ca2+ transport ATPase (SERCA), a known target for the development of novel therapeutics for rheumatoid arthritis. Additionally, the drug-likeness of the synthesized compound was assessed by predicting its pharmacokinetic properties.
{"title":"(2R,4aS,6aS,12bR,14aS,14bR)-N-(2-(2-(2-(2-Azidoethoxy)ethoxy)ethoxy)ethyl)-10-hydroxy-2,4a,6a,9,12b,14a-hexamethyl-11-oxo-1,2,3,4,4a,5,6,6a,11,12b,13,14,14a,14b-tetradecahydropicene-2-carboxamide","authors":"Guo Yuzhu, Margrate Anyanwu, Xiao Yang, Ren Zimo, Alessandra Gianoncelli, Giovanni Ribaudo, P. Coghi","doi":"10.3390/m1800","DOIUrl":"https://doi.org/10.3390/m1800","url":null,"abstract":"In this report, we discuss the synthesis of a compound obtained from the derivatization of the natural compound celastrol. This derivative is connected to PEG azide moiety through an amide linkage. The linkage was achieved through the activation of the carboxylic acid using HOBt/EDC. The compound was fully characterized by proton (1H), carbon-13 (13C), heteronuclear single quantum coherence (HSQC), correlation spectroscopy (1H-1H-COSY), and distortionless enhancement by polarization transfer (DEPT) NMR. Ultraviolet (UV), Fourier-transform infrared (FTIR), and high-resolution mass spectrometry (HRMS) were also adopted. Computational investigations were conducted to forecast the binding mode between the synthesized compound and sarco-endoplasmic reticulum (SR) Ca2+ transport ATPase (SERCA), a known target for the development of novel therapeutics for rheumatoid arthritis. Additionally, the drug-likeness of the synthesized compound was assessed by predicting its pharmacokinetic properties.","PeriodicalId":509184,"journal":{"name":"Molbank","volume":"137 ","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140767169","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}
The previously unknown cyclopropane spiro-fused with isoxazol-5-one ((1RS,3SR)-1-(4-methylbenzyl)-7-phenyl-5-oxa-6-azaspiro[2.4]hept-6-en-4-one) was synthesized from benzylideneisoxazol-5-one in 34% yield via double methylene transfer from diazomethane. The structure of the compound was established based on 1H, 13C, and 2D NMR spectroscopy and high-resolution mass spectrometry, and confirmed by X-ray diffraction analysis.
通过二氮甲烷的双亚甲基转移，从苯亚甲基异恶唑-5-酮合成了之前未知的环丙烷螺融合异恶唑-5-酮（(1RS,3SR)-1-(4-甲基苄基)-7-苯基-5-氧杂-6-氮杂螺[2.4]庚-6-烯-4-酮），收率为 34%。根据 1H、13C 和 2D NMR 光谱法和高分辨率质谱法确定了该化合物的结构，并通过 X 射线衍射分析予以证实。
{"title":"(1RS,3SR)-1-(4-Methylbenzyl)-7-phenyl-5-oxa-6-azaspiro[2.4]hept-6-en-4-one","authors":"Gleb D. Titov, N. Rostovskii","doi":"10.3390/m1799","DOIUrl":"https://doi.org/10.3390/m1799","url":null,"abstract":"The previously unknown cyclopropane spiro-fused with isoxazol-5-one ((1RS,3SR)-1-(4-methylbenzyl)-7-phenyl-5-oxa-6-azaspiro[2.4]hept-6-en-4-one) was synthesized from benzylideneisoxazol-5-one in 34% yield via double methylene transfer from diazomethane. The structure of the compound was established based on 1H, 13C, and 2D NMR spectroscopy and high-resolution mass spectrometry, and confirmed by X-ray diffraction analysis.","PeriodicalId":509184,"journal":{"name":"Molbank","volume":"92 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-04-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140785676","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}
Bakr F. Abdel-Wahab, Hanan A. Mohamed, B. Kariuki, Gamal A. El-Hiti
The reaction of equimolar quantities of 3-(1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazol-4-yl)-1-phenyl-1H-pyrazole-4-carbaldehyde and (2,4,6-trichlorophenyl)hydrazine in ethanol containing concentrated hydrochloric acid (0.2 mL; 37%) as a catalyst under reflux for 2 h yielded 1-(1-(benzofuran-2-yl)ethylidene)-2-(2,4,6-trichlorophenyl)hydrazine. The crude produced was purified by crystallization using dimethylformamide to provide the title heterocycle in a 95% yield. The structure of the newly synthesized heterocycle was confirmed through X-ray diffraction and spectral analyses.
{"title":"(E)-1-(4-Methoxyphenyl)-5-methyl-4-(1-phenyl-4-((2-(2,4,6-trichlorophenyl)hydrazineylidene)methyl)-1H-pyrazol-3-yl)-1H-1,2,3-triazole","authors":"Bakr F. Abdel-Wahab, Hanan A. Mohamed, B. Kariuki, Gamal A. El-Hiti","doi":"10.3390/m1798","DOIUrl":"https://doi.org/10.3390/m1798","url":null,"abstract":"The reaction of equimolar quantities of 3-(1-(4-methoxyphenyl)-5-methyl-1H-1,2,3-triazol-4-yl)-1-phenyl-1H-pyrazole-4-carbaldehyde and (2,4,6-trichlorophenyl)hydrazine in ethanol containing concentrated hydrochloric acid (0.2 mL; 37%) as a catalyst under reflux for 2 h yielded 1-(1-(benzofuran-2-yl)ethylidene)-2-(2,4,6-trichlorophenyl)hydrazine. The crude produced was purified by crystallization using dimethylformamide to provide the title heterocycle in a 95% yield. The structure of the newly synthesized heterocycle was confirmed through X-ray diffraction and spectral analyses.","PeriodicalId":509184,"journal":{"name":"Molbank","volume":"46 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2024-03-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"140371582","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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