详细信息
文献类型:期刊文献
中文题名:氟丙嘧草酯的合成新工艺
英文题名:A Novel Process for Synthesis
作者:李爱军[1];廖道华[1];高倩[1];郭栋[1];陈立鹏[1]
机构:[1]华东理工大学药学院,上海200237
年份:2015
卷号:23
期号:4
起止页码:358
中文期刊名:合成化学
外文期刊名:Chinese Journal of Synthetic Chemistry
收录:CSTPCD;;CSCD:【CSCD_E2015_2016】;
语种:中文
中文关键词:氟丙嘧草酯;2-氯-5-硝基苯甲酸甲酯;除草剂;药物合成
外文关键词:Butafenacil; methyl 2-chloro-5-(ethoxycarbonylamino) benzoateuracil; herbicide; drug synthesis
摘要:以2-氯-5-硝基苯甲酸甲酯为原料,经还原、缩合得2-氯-5-(乙氧羰基)氨基苯甲酸甲酯(3);3与3-氨基-4,4,4-三氟巴豆酸乙酯进行环合得脲嘧啶环中间体(4);4经甲基化、水解、酰化和缩合反应合成了氟丙嘧草酯,总收率55.2%,纯度99.1%。中间体和产物结构经1H NMR和EI-MS确证。
Methyl 2-chloro-5-(ethoxycarbonylamino) benzoate(3) was obtained by reduction and condensation reaction using methyl 2-chloro-5-nitrobenzoate as the material.Butafenacil in total yield of 55.2% with 99.1% purity was synthesized by cyclization reaction of 3 with(Z)-ethyl 3-amino-4,4,4-trifluorobut-2-enoate,and then through methylation,hydrolysis,acylation and consideration.The structures of products and intermediates were confirmed by1 H NMR and EI-MS.
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