Buclizine drug intermediates 4-tert-butyl-benzyl chloride synthesis method

摘要

#$%^&*AU2016102298A420170223.pdf#####ABSTRACT Buclizine drug intermediates 4-tert-butyl-benzyl chloride synthesis method, comprising the following steps: equipped with a stirrer, a thermometer, a dropping funnel, the reaction vessel, was added 1.6mol tert-butylbenzene (2), 530ml chloroethane (3) was added, 2.1-2.3mol methylamine (4) was added, 1.6mol chloro cuprous, 310ml oxalic acid solution, stirring speed was controlled at 150-190rpm, elevated the solution temperature at 70-75 C , 210ml cyclohexane was added, continued to stirring the reaction for 10-13h after addition, reducing the solution of temperature to 40--45 C, separated the oil layer, washed with salt solution, potassium sulfite solution, dehydrated with dehydrating agent, vacuum distillation, collecting fractions of 90--95 C, recrystallized in toluene solution, got 4-tert-butylbenzyl chloride.