对氟苯甲醛的合成研究  

Study on Synthesis of P- fluorobenzaldehyde

作　　者：苟蓓蕾 傅颖[1] 田新新[1] 刘晓彬[1] 沈彤[1] 

机构地区：[1]兰州交通大学,甘肃兰州730070

出　　处：《广州化工》2016年第12期97-98,137,共3页GuangZhou Chemical Industry

摘　　要：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1HNMR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。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 by1 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%.

关 键 词：4-氟苯甲醛 4-氟氯化苄 乌洛托品 醋酸锌 

分 类 号：O625.44[理学—有机化学]