硼酸酯催化合成2-羟基-4-甲氧基二苯甲酮

Synthesis of 2-Hydroxy-4-methoxybenzophenone Catalyzed by N-Octyldiethanolamine Borate

以2,4 二羟基二苯甲酮及硫酸二甲酯为原料,用自制的N 正辛基硼酸二乙醇胺酯为催化剂合成了2 羟基 4 甲氧基二苯甲酮,研究了原料摩尔比、催化剂用量、反应时间、反应温度等因素对产品的影响。实验表明,在n(2,4 二羟基二苯甲酮)∶n(硫酸二甲酯)=1∶0 55,m(N 正辛基硼酸二乙醇胺酯)/m(2,4 二羟基二苯甲酮)=0 02,反应温度70℃,反应时间4h的条件下,w(2 羟基 4 甲氧基二苯甲酮)=98 8%,w(2,4 二甲氧基二苯甲酮)<0 8%,收率达94 6%。

2-Hydroxy-4-methoxybenzophenone(Ⅰ) was synthesized from 2,4-dihydroxybenzophenone(Ⅱ) and dimethyl sulfate(Ⅲ) in the presence of N-octyldiethanolamine borate(Ⅳ).The optimal reaction conditions were n(Ⅱ)∶n(Ⅲ)=1∶0.55,m(Ⅳ)/m(Ⅱ)=0.02,reaction temperature 70 ℃ and reaction time 4 h.Yield of Ⅰ was 94.6% with 98.8% purity and the content of 2,4-dimethoxybenzophenone < 0.8%.