摘要
以甲氰菊酸乙酯为起始原料,经皂化、酸化和酰氯化反应制取了2,2,3,3-四甲基环丙烷基酰氯,确定各步反应操作中适宜的工艺条件如下:甲氰菊酸乙酯与NaOH的物质的量比为1:4,皂化时间为8~10h,酸化温度为60~65℃,甲氰菊酸与SOCl_2物质的量比为1:1.2,酰氯化反应温度为45~55℃,反应时间约为6h。中试结果表明,工艺操作平稳,产品质量稳定,适合工业化生产。
2,2,3,3 -Tetramethylcyclopropanyl chloride was prepared through the successive processes of saponification, acidification and acyl chlorination with 2,2,3,3 -tetramethylcyclopropane carboxylic ethyl ester as the starting material, and the appropriate reaction conditions in the processes are identified, i.e. the quantity ratio of 2,2,3,3 - tetramethylcyclopropane carboxylic ethyl ester to NaOH: 1:4, saponification time : 8 - 10 h, acidification temperature: 60 -65℃, the quantity ratio of 2,2,3,3 - tetramethylcyclopropane carboxylic ethyl ester to SOCl2 : 1 : 1.2, acyl chlorination reaction temperature : 45 - 55 ℃, reaction time : =6 h. The results of pilot test have shown that the process operation is smooth, and the product quality is stable, indicating that this technique can be put into commercial application.
出处
《精细石油化工进展》
CAS
2011年第6期42-44,共3页
Advances in Fine Petrochemicals
关键词
2
2
3
3-四甲基环丙烷基酰氯
甲氰菊酸乙酯
合成
中试
2,2,3,3 - tetramethylcyclopropanyl chloride
2,2,3,3 - tetramethylcyclopropane carboxylic ethyl ester
synthesis
pilot test