邻氟苯酚是一种重要的医药和农产化学品的中间体,用于合成杀菌剂、除草剂,也可合成染料液晶、塑料及橡胶的添加剂等。主要以邻氟苯胺为原料,经微通道重氮,水解反应得到邻氟苯酚。系统研究了重氮反应温度、反应停留时间、硫酸用量、亚硝...邻氟苯酚是一种重要的医药和农产化学品的中间体,用于合成杀菌剂、除草剂,也可合成染料液晶、塑料及橡胶的添加剂等。主要以邻氟苯胺为原料,经微通道重氮,水解反应得到邻氟苯酚。系统研究了重氮反应温度、反应停留时间、硫酸用量、亚硝酸钠用量、催化剂、水解温度、水解酸浓度等因素对反应工艺的影响。重氮优化工艺为:硫酸与邻氟苯胺当量为6∶1,亚硝酸钠与邻氟苯胺当量为1.1∶1,重氮反应温度60℃,重氮停留时间32.7 s (持液体积27 m L);水解优化工艺为:水解温度185℃,催化剂硫酸铜用量为原料重量的10%,水解酸浓度40%最佳,最后邻氟苯酚收率可以达到90%。展开更多
Pentaflurophenyl acrylates were synthesized for the first time via the condensation reaction of acrylic acids with pentaflurophenol by using N,N’-dicyclohexylcarbodiimide(DCC)as condensing agent,and good yields(74-81...Pentaflurophenyl acrylates were synthesized for the first time via the condensation reaction of acrylic acids with pentaflurophenol by using N,N’-dicyclohexylcarbodiimide(DCC)as condensing agent,and good yields(74-81%)were obtained.The structures of products were confirmed by 1H NMR and ES-MS.展开更多
文摘邻氟苯酚是一种重要的医药和农产化学品的中间体,用于合成杀菌剂、除草剂,也可合成染料液晶、塑料及橡胶的添加剂等。主要以邻氟苯胺为原料,经微通道重氮,水解反应得到邻氟苯酚。系统研究了重氮反应温度、反应停留时间、硫酸用量、亚硝酸钠用量、催化剂、水解温度、水解酸浓度等因素对反应工艺的影响。重氮优化工艺为:硫酸与邻氟苯胺当量为6∶1,亚硝酸钠与邻氟苯胺当量为1.1∶1,重氮反应温度60℃,重氮停留时间32.7 s (持液体积27 m L);水解优化工艺为:水解温度185℃,催化剂硫酸铜用量为原料重量的10%,水解酸浓度40%最佳,最后邻氟苯酚收率可以达到90%。
文摘Pentaflurophenyl acrylates were synthesized for the first time via the condensation reaction of acrylic acids with pentaflurophenol by using N,N’-dicyclohexylcarbodiimide(DCC)as condensing agent,and good yields(74-81%)were obtained.The structures of products were confirmed by 1H NMR and ES-MS.