摘要
以3-甲基-2-硝基苯甲酸为原料通过RaneyNi加氢还原制得3-甲基-2-氨基苯甲酸,接着与N-氯代丁二酰亚胺(NCS)反应制得3-甲基-2-氨基-5-氯苯甲酸,然后3-甲基-2-氨基-5-氯苯甲酸与氯化亚砜在75～80℃下回流3h后,接着缓慢滴加甲胺水溶液,在室温下搅拌反应12h,得到2-氨基-5-氯-N,3-二甲基甲酰胺。然后再与3-溴-1-(3-氯吡啶-2-吡啶基)-1 H-吡唑-5-甲酸在-5～0℃下滴加甲基磺酰氯反应得到产品氯虫苯甲酰胺,四步总收率37.0%,产品HPLC纯度是96.05%。
2-Amino-3-methylbenzoic acid was synthesized by hydrogenation of 3-methyl-2-nitrobenzoic acid using RaneyNi as catalyst.2-Amino-5-chloro-3-methylbenzoic acid was prepared from 2-amino-3-methylbenzoic acid and N-chlorosuccinimid（NCS）.2-Amino-5-chloro-N,3-dimethylbenzamide was prepared from aqueous methylamine solution and the intermediate which was synthesized by the reaction of 2-amino-5-chloro-3-methylbenzoic acid and thionyl chloride at 75~80℃ for 3 h.Chloranthraniliprole was prepared from 2-amino-5-chloro-N,3-dimethylbenzamide and 3-bromo-1-（3-chloro-2-pyridinyl）-1H-pyrazole-5-carboxylic acid by dropping methanesulfonyl chloride at-5~0℃.The total yield was 37.0% and the purity of the product was 96.05%.
出处
《化学世界》
CAS
CSCD
北大核心
2012年第10期612-614,628,共4页
Chemical World
