| 摘要 |
Tamoxifen drug intermediates epibromohydrin synthesis method, comprising the following steps: equipped with distillation apparatus, the reaction vessel was added 5.6mol 1-amino-3-bromo-propanol(2), 6.1-6.3mol 2-bromo-phenol solution(3), 800ml potassium bromide solution, 2.56mol alumina, 700ml hexane solution, 300ml sodium sulfite solution, rising the solution temperature to 70-75 0C, keeping reaction 3-5h, reducing the temperature of the solution to 50-550 C, controlling the stirring speed 110-150rpm, refluxed for 90-110min, reduced solution temperature to 10-13 0C, allowed to stand for 2-5h, layers were separated and removed the oil layer, washed with salt solution, washed with acetonitrile solution, washed with isopropanol solution, vacuum distillation, collecting fractions of 80-850C, recrystallization in nitromethane solution , got crystal epibromohydrin. |
