摘要
[目的]优化并改进茚草酮的合成工艺。[方法]以间溴氯苯为原料,经格氏反应、氯代反应生成关键中间体1-氯-3-(3-氯丙-1-烯-2-基)苯。在氢钠存在的条件下,邻苯二甲酸二乙酯与乙酸丁酯反应得到2-乙基-1H-茚-1,3(2H)-二酮。最后,1-氯-3-(3-氯丙-1-烯-2-基)苯与2-乙基-1H-茚-1,3(2H)-二酮发生取代反应、经环氧化反应得到目标产物茚草酮。[结果]在优化的反应条件下,总收率为44.2%。[结论]该工艺收率高、操作简便、产品纯度高,适合工业化生产。
[Aims]This paper aims to optimize and improve the synthetic process for indanofan.[Methods] With 1 -bromo-3-chlorobenzene as a starting material, reacted via Grignard reaction and chlorination reaction to obtain the key intermediate of 1 -chloro-3-(3-chloroprop-1 -en-2-yl) benzene. In the presence of sodium hydride, diethyl phthalate reacted with ethyl butyrate to obtain 2-ethyl-1H-indene-1,3(2H)-dione. At last, 2-ethyl-1H-indene-1,3(2H)-dione take place substitution reaction with 1 -chloro-3-(3-chloroprop-1-en-2-yl) benzene and via epoxidation reaction to obtain the target product indanofan.[Resul⑸ Under the optimal conditions, the total yield was 44.2%.[Conclusions]The process has the advantages of high yield, simple operation and high purity, which is suitable for industrial manufacture.
作者
杜蔚
任春阳
宋巍
周雅婷
付德才
冯雪
DU Wei;REN Chun-yang;SONG Wei;ZHOU Ya-ting;FU De-cai;FENG Xue(Hebei University of Science and Technology, Shijiazhuang 050018, China)
出处
《农药》
CAS
CSCD
北大核心
2019年第3期177-179,共3页
Agrochemicals
关键词
茚草酮
除草剂
合成
indanofan
herbicide
synthesis