奈韦拉平中间体的制备工艺  

Study on the Preparation Process of Nevirapine Intermediate

作　　者：丁永山 王文魁 王福军 杜翔 蒋建华 甘华军 岳瑞宽 陈洪龙 Ding Yongshan;Wang Wenkui;Wang Fujun;Du Xiang;Jiang Jianhua;Gan Huajun;Yue Ruikuan;Chen Honglong(Nanjing Red Sun Biochemistry Co.,Ltd.,Nanjing 210047,China)

机构地区：[1]南京红太阳生物化学有限责任公司,江苏南京210047

出　　处：《山东化工》2024年第3期57-60,共4页Shandong Chemical Industry

摘　　要：以2,6-二氯-4-甲基吡啶为原料,经硝化反应,“一锅法”选择性还原、脱氯步骤即可得2-氯-3-氨基-4-甲基吡啶。分别考察了传统的混酸硝化和微通道反应器硝化反应;“一锅法”选择性还原、脱氯反应采用威尔金森催化剂,该催化剂具有选择性高、稳定性好、可多次重复套用的优点。最佳的硝化反应条件采用微通道反应器、反应温度15℃、停留时间60 s,发烟硝酸和2,6-二氯-4-甲基吡啶物质的量比1.2∶1,收率可达93%;最佳的“一锅法”条件为催化剂添加量1.2%,反应温度90℃,压力1.1 MPa,收率92%。Using 2,6-dichloro-4-methylpyridine as raw material,2-chloro-3-amino-4-methyl pyridine can be obtained through nitration reaction,and"one-pot method"which including the selective reduction and dechlorination.The nitration reactions through traditional method of mixed acid and micro-channel reactor have been investigated respectively.Wilkinson catalyst has been used in the selective reduction and dechlorination which were names as"one-pot method".This catalyst has the advantages of high selectivity,good stability and repeated application.The optimum nitrification conditions were micro-channel reactor,reaction temperature was 15℃,residence time was 60 seconds,the molar ratio of fuming nitric acid to 2,6-dichloro-4-methyl was 1.2∶1,and the yield was 93%.The optimum conditions of"one-pot method"were as below:the amount of catalyst added was 1.2%,reaction temperature was 90℃,pressure was 1.1 MPa and the yield was 92%.

关 键 词：混酸硝化 微通道反应器 选择性还原 威尔金森催化剂 

分 类 号：TQ253.2[化学工程—有机化工]