摘要
在季铵盐四乙基溴化铵存在下，３，４－亚甲二氧基正丙基苯进行氯甲基化反应的转化率达９６．６％，定位选择性达１００％。对产物进行了气相色谱、红外光谱、核磁共振测定及元素分析。
Improved yield and selectivity for the chloromethylation of a 3,4 methylenedioxy propylbenzene(dihydrosafrole) in the presence of a phase transfer catalyst tetraethylammonium bromide are reported. To find the optimal reaction comditions, an orthogonality experiment designed by L 9(3 4) Form with three factors and three levels, was carried out. The results showed that the temperature had the biggest influence on the reaction yield, and the amount of catalyst had the lowest influence. The optimal technology was: dihydrosafrole 1 mole, 37% formaldehyde solution 2.0 mole, 37% concentrated hydrochloric acid 2.0 mole, catalyst 3g, for a period of about 16 hours at a temperature 50℃. In this new technology, the mole number of formaldehyde and hydrochloric acid was only half of that used in the known technology the yield of chloromethylation was increased by 23.6%.
出处
《合成化学》
CAS
CSCD
1997年第2期202-204,共3页
Chinese Journal of Synthetic Chemistry
基金
湖南省科委科技基金
关键词
亚甲二氧基
正丙基苯
胡椒基丁醚
氯甲基化
Dihydrosafrole, Piperonyl butoxide, Chloromethylation, Phase transfer catalysis.
