2,3-二氯吡啶的合成新工艺

李爱军, 徐朝洁, 张志伟
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Abstract

为满足市场需求,对2 ,3-二氯吡啶的合成工艺进行了研究.以2-氯烟酸为起始原料,经酰胺化、霍夫曼(Hofm ann)酰胺降解、重氮化和Sandmeyer 4 步反应,得到2 ,3-二氯吡啶,对影响产率的因素(如PC13 用量、NaOH 浓度、反应温度、催化剂用量)进行了优化.结果表明:酰胺化中,n(2 -氯烟酸):w(PCl3) = l : 0.45 ;霍夫曼降解反应中,NaOH 质量分数为18% ,反应温度为75?80°C;Sandmeyer反应中,n (2-氯-3-氨基p比咬):n (氧化铜)= 1 : 0. 3.在此优化条件下,反应总收率为70. 33% (以2-氯烟酸计),纯度达98. 5% ,通过1 H -N M R 进行了结构表征.此法产品纯度高,操作简便,原料易得.
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2,3-二氯吡啶的合成新工艺
为满足市场需求,对2 ,3-二氯吡啶的合成工艺进行了研究.以2-氯烟酸为起始原料,经酰胺化、霍夫曼(Hofm ann)酰胺降解、重氮化和Sandmeyer 4 步反应,得到2 ,3-二氯吡啶,对影响产率的因素(如PC13 用量、NaOH 浓度、反应温度、催化剂用量)进行了优化.结果表明:酰胺化中,n(2 -氯烟酸):w(PCl3) = l : 0.45 ;霍夫曼降解反应中,NaOH 质量分数为18% ,反应温度为75?80°C;Sandmeyer反应中,n (2-氯-3-氨基p比咬):n (氧化铜)= 1 : 0. 3.在此优化条件下,反应总收率为70. 33% (以2-氯烟酸计),纯度达98. 5% ,通过1 H -N M R 进行了结构表征.此法产品纯度高,操作简便,原料易得.
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期刊介绍: Journal of Hebei University of Science and Technology is a comprehensive academic science and technology journal hosted by Hebei University of Science and Technology, which is openly distributed at home and abroad, published bimonthly at the end of each month, with the domestic uniform serial number CN 13-1225/TS and the international standard serial number ISSN 1008-1542. It is selected as one of the Chinese core journals of Peking University, Chinese core journals of science and technology, RCCSE Chinese core academic journals (A), excellent scientific and technological journals of Chinese colleges and universities, and ‘Top Ten’ journals of Hebei Province. According to the ‘Annual Report on Impact Factor of Chinese Academic Journals (2024 Edition)’ issued by China Knowledge Evaluation Centre in October 2024, the compound impact factor of Journal of Hebei University of Science and Technology is 1.736 (35/146 in subject order), and the influence index (CI) is 336 (62/146 in subject order). Journal of Hebei University of Science and Technology mainly publishes research papers in the fields of [Mechanical, Electronic and Information Science], [Material Science], [Food and Biological Science], [Textile Science], [Civil and Architectural Engineering], [Transportation and Logistics], etc. It also has [National Youth/Regional Science Fund Project Columns ], [Chemistry and Chemical Industry Column], [New Energy and Energy Conservation and Environmental Protection Column], [Data Analysis and Calculation Column] and [Xiongan Green Innovation Column] 5 special columns. Journal of Hebei University of Science and Technology is now published in China Academic Journals Network Publishing Database (China Knowledge), ‘China Science and Technology Paper Statistics Source Journal’ (China Science and Technology Core), Chinese Science and Technology Journal Database (Wipo), Wanfang Database, Changjiang Literature Library, Taiwan Chinese Journal Database, Chinese Journal Database, Chinese Journal Database, Chinese Journal Database, Chinese Journal Database, Chinese Journal Database, and Chinese Journal Database. Database, Changjiang Literature Library, Chinese Electronic Periodical Service in Taiwan - CEPS (CEPS), as well as the American Chemical Abstracts (Web Edition) (CA), the American Ulrich's Journal Guide (Web Edition) (Ulrichsweb), the American EBSCOhost Database (EBSCO), the British Polymer Library (PL), DOAJ (Sweden), HINARI (Switzerland), and JSTChina (Japan Science and Technology Agency).
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