摘要
以三氟甲基苯为起始原料 ,经硝化和常压催化加氢制备间三氟甲基苯胺 ,总收率达 89% ,纯度 99%以上。硝化反应的优化条件为 :n(PhCF3 )∶n(HNO3 )∶n(H2 SO4) =1∶1.0 5∶1.3,间三氟甲基硝基苯收率 90 .7% ,纯度 98.0 % ;最佳氢化条件 :催化剂用量 2 % ,原料配比为 0 .10mol间三氟甲基硝基苯 / 10 0mL无水乙醇 ,氢化温度 4 5℃ ,搅拌速度 2 4 0r/min ,间三氟甲基苯胺收率 98.5 % ,纯度 99.3%。
m -Trifluoromethylaniline was prepared from benzotrifluoride (phCF_3) by nitration and normal pressure catalytic hydrogenation. The purity was above 99% and the total yield reached to 89%. The optimum ratio of nitrating agent is PhCF_3∶HNO_3∶H_2SO_4=1∶1.05∶1.3(mol), the purity and yield of m -trifluoromethyl nitrobenzene were 98.0% and 90.7% respectively. The optimum conditions of catalytic hydrogenation are as follows: weight of 5% Pd/C catalyst used in the substrate=2%, trifluoromethyl nitrobenzene∶absolute ethanol=0.10 mol∶100 mL, reaction temperature 45 ℃, stirring speed 240 r/min, the purity and the yield of m -trifluoromethylaniline were 99.3% and 98.5% respectively.
出处
《精细石油化工》
CAS
CSCD
北大核心
2003年第1期40-43,共4页
Speciality Petrochemicals
