奈韦拉平中间体的制备工艺
Study on the Preparation Process of Nevirapine Intermediate
丁永山 1王文魁 1王福军 1杜翔 1蒋建华 1甘华军 1岳瑞宽 1陈洪龙1
作者信息
- 1. 南京红太阳生物化学有限责任公司,江苏 南京 210047
- 折叠
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%.
Abstract
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Key words
mixed acid nitration/microchannel reactor/selective reduction/Wilkinson catalyst引用本文复制引用
出版年
2024
NETL
NSTL
万方数据