摘要
以冰乙酸为溶剂,以5-叔丁基-2-羟基苯甲醛和溴素为原料,合成了3-溴-5-叔丁基-2-羟基苯甲醛。考察了溶剂、反应温度、物料比、反应时间等对3-溴-5-叔丁基-2-羟基苯甲醛收率的影响,合成的优化工艺条件为:n(5-叔丁基-2-羟基苯甲醛)∶n(溴素)=1∶1.1,反应温度60℃,反应时间10 h,在此工艺下,收率可达到88.2%,产品经MS、1H NMR确认。
3-Bromo-5-tert-butyl-2-hydroxy-benzaldehyde(BTHB)was synthesized from bromine and 5-tert-butyl-2-hydroxy-benzaldehyde(THB)in 88.2% yield in acetic acid.The reaction conditions were investigated and the optimal conditions were as followings:solvent of acetic acid,molar ratio of THB to bromine of 1.1 to 1,temperature of 60℃,reaction time of 10 h.The final product was characterized with 1H NMR.
出处
《精细化工中间体》
CAS
2012年第3期17-20,共4页
Fine Chemical Intermediates
基金
中科院知识创新重要方向性项目(KZCX2-YW-412)
唐山市科技局项目(1016021A-7)