摘要
研究了以2,4二氟苯胺为原料,经芳烃偶联反应、傅- 克酰化反应、拜耳- 维利格反应、水解反应、羧化反应来合成氟苯水杨酸这一工艺路线。得到了各步反应的最佳反应条件:偶联反应的最佳反应温度为10℃,酰化反应中n(三氯化铝)∶n (联苯) =2-6∶1,氧化反应应在惰性反应环境和催化剂催化的条件下进行,过酸与芳酮的最佳物质的量比为3-0∶1,惰性气体保护和惰性反应介质有利于羧化反应的进行。在新的工艺条件下单程总收率达到42-5% 。
The title compound was synthesized from 2,4 difluoroaniline by five reactions such as arylation,Friedel Crafts acylation, Baeyer Villiger reaction,saponification and carbonation.The best technological parameters of each reaction were got as follows:the temperature of arylation was 10℃,in acylation the molar ratio of AlCl 3 to biphenyl was about 2 6/1 ,in oxidation the molar ratio of RCO 3H/ArCOR should be 3 0/1,catalyst,nitrogen atmosphere and two stage operation were very important to the oxidation reaction.The overall yield was about 42 5%.
出处
《精细化工》
EI
CAS
CSCD
北大核心
1999年第6期19-21,共3页
Fine Chemicals