摘要
以邻甲氧基苯乙烯为原料,先进行二氯加成反应,然后与丙二酸二乙酯进行环丙烷基化反应,再通过Krapcho脱酯基反应,最后在碱性条件下用苯硫酚去甲基化形成新型烟用香料2-(邻羟基苯基)环丙烷-1-甲酸,总收率达61%。目标化合物通过核磁、质谱进行了表征。该路线反应条件温和、试剂廉价易得且收率高,为其工业化合成提供了参考。
2-( 2-Hydroxyphenyl ) cyclopropane-l-carboxylic acid (, HEIA ) was preparea irom the starting material of 2-methoxystyrene via the chlorine-addition, eyelopropanation reaction with diethyl malonate, Krapcho decarboxylation and demethylation using thiophenol as nueleophiles under alkali conditions with a high total yield of 61%. The target product was also confirmed through tHNMR, t3 CNMR, GC-MS and HRMS. The synthetic process of HCCA can be performed under mild reaction conditions with conveniently available reagents and good yields, providing a potential route for the large scale syntheses.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2013年第11期1234-1236,1246,共4页
Fine Chemicals