摘要 |
Naftifine drug intermediates N- methyl-i -naphthalene methylamine synthesis method, comprising the following steps: equipped with a stirrer, a thermometer, a condenser and a dropping funnel, the reaction vessel was added 130ml propionitrile solution, 210ml methyl amine (3), reducing the solution temperature to 13-16 C, controlling the stirring speed 110-130rpm, 0.31mol amine methyl naphthalene(2) was added slowly, controlled dropping time in 3-4h, elevated the solution temperature to 40-45 C, standing for 30-36h, evaporated propionitrile , the residue was added 230ml cyclohexane solution, successively washed with potassium bisulfite solution, washed with salt solution, dehydrated with dehydration agent, vacuum distillation, collecting fractions of 110--115 C, recrystallized from nitromethane solution, got N methyl-1 -naphthalene methanamine crystals . |