钛酸四丁酯催化合成硝基卡因的研究

Catalytic Synthesis of Diethylamonoethyl p-Nitrobenzoate by Tetrabutyl Titanate

对硝基苯甲酸和N,N-二乙基乙醇胺在二甲苯溶液中,以直接酯化法合成硝基卡因。通过对催化剂种类、催化剂用量、反应时间等影响因素的考察,确定以钛酸四丁酯作为催化剂,催化剂用量为对硝基苯甲酸质量的3.5%,n(对硝基苯甲酸)∶n(N,N-二乙基乙醇胺)=1∶1,反应14h。硝基卡因的产率达到82.1%,比没有催化剂时产率提高11.8%。

Diethylaminoethyl p-nitrobenzoate was synthesized by direct catalytic esterification of p-nitrobenzoic acid and diethylaminoethanol. The optimized reaction conditions were determined, including the type and the amount of catalyst along with reaction time. Tetrabutyl titanate was chosen as the best catalyst while the optimal conditions were follows: the amount of used catalyst equaled to 3.5% of the amount of p-nitrobenzoic acid while the molar ratio of diethylaminoethanol to p-nitrobenzoic acid was 1∶1. After reaction of 14 h, the yield of diethylaminoethyl p-nitrobenzoate reached 82.1%, about 11.8% higher than that in the reaction without catalyst.