对氟苯甲醛的合成研究

摘要

With 4-fluoro-benzyl chloride and hexamine as raw materials in the presence of acetic acid and zinc acetate, 4-fluorobenzaldehyde was synthesized by “one-pot” sommelet reaction and the structure and purity of product were determined by 1 HNMR and HPLC. The amount of methenamine, the amount of catalyst zinc acetate, the amount of acetic acid, reaction time and other reaction conditions were optimized. Results showed that n(4-fluorobenzyl chloride):n(acetic acid):n(methenamine)=1:2. 5:1. 6, catalyst was 0. 05 eq of 4-fluorobenzyl chloride, reaction temperature was 80 ℃, reaction time was 3 h. The maximum yield of product was up to 92%, purity was more than 94%.%以对氟氯化苄与乌洛托品为原料,在醋酸和醋酸锌的存在下,利用sommelet反应,“一锅法”合成了对氟苯甲醛,并通过1 HNMR和HPLC对产物结构和纯度进行了确定,对乌洛托品用量,催化剂醋酸锌用量,醋酸用量,反应时间等反应条件进行了筛选优化,结果显示： n(对氟氯化苄)：n(乙酸)：n(乌洛托品)=1：2．5：1．6,催化剂为对氟氯化苄的0．05 eq,温度为80℃,反应时间为3 h时,得到产物的最高收率达到96%,纯度可达94%以上。