邻氟苯甲腈的合成研究

以邻甲苯胺为原料 ,采用四步反应法合成邻氟苯甲腈。 (1)邻甲苯胺经西曼反应合成邻氟甲苯 ,收率 6 5 % ;(2 )邻氟甲苯经氯化、水解得到邻氟苯甲醛 ,以过氧化苯甲酰为氯化引发剂 ,氧化锌为水解催化剂 ,收率 80 % ;(3)邻氟苯甲醛经肟化反应得到邻氟苯甲醛肟 ,收率 87% ;(4)肟用乙酸酐脱水合成出邻氟苯甲腈 ,收率 76 % ,产品质量分数大于 99%。

Synthesis of o-Fluorobenzonitrile

o Fluorobenzonitrile was synthesized in four step reaction with o-tolidine as raw material. (1) o Fluorotoluene (Ⅰ) was prepared from o-tolidine through Schiemann reaction in 65% yield. (2) o Fluorobenzaldehyde (Ⅱ) was prepared fromⅠthrough chlorination and hydrolysis reactions in 80%yield with benzoyl peroxides as chloridination catalyst and zinc oxide as hydrolysis catalyst.(3) o Fluorobenzaldoxime (Ⅲ) was obtained by oximation ofⅡin 87% yield.(4) o Fluorobenzonitrile was obtained from Ⅲ by dehydration reaction with acetic anhydride as dehydrating reagent in 76% yield and of 99% purity.