肼基碳酸苄酯合成工艺研究

Study on the Synthesis Process of Benzyl Carbazate

研究了以DMC、苯甲醇为原料,碳酸钠为催化剂,先合成碳酸二苄酯,然后碳酸二苄酯再与水合肼反应,制得肼基碳酸苄酯。通过设计正交实验考查了物料配比、反应时间、反应温度、催化剂用量等因素对反应的影响,确定了合成中较佳的实验条件:DMC、苯甲醇、水合肼的摩尔比为1.0:2.0:1.6,催化剂碳酸钠用量为DMC质量的3.3%,第一步反应温度为140℃,时间为4h;第二步反应温度为130℃,时间为4h。产品经质谱(MS)分析与目的产物相一致。

Benzyl carbazate was synthesized by reaction of hydrazine hydrate and dibenzyl carbonate which synthesized by DMC and benzyl alcohol and catalysed by sodium carbonate. Through designing orthogonal experiment, the effect factors, such as the mol ratio of raw materials, reaction time, reaction temperature, catalytic quantity, etc., were investigated to find the preferred reaction conditions. The first reaction was carried out at 140℃ for 4h, while the second reaction at 130℃ for 4h. The mol ratio of dimethyl carbonate, benzyl alcohol and hydrazine hydrate was 1.0：2.0：1.6, and the weight ratio of catalyst sodium carbonate to dimethyl carbonate was 3.3%. The MS spectrogram of the product agreed with the target product.