| 摘要 |
Osalmide drug intermediates N- p-hydroxyphenyl salicylamide synthesis method, comprising the following steps: the reaction vessel was added 0.07 mol p-aminophenol (3), 0.074-0.076mol 2- hydroxy benzamide (2), 70- 80ml ethyl acetate, controlling the stirring speed 110-150rpm, slowly added 0.031 mol stannous chloride , when color of the solution became dark, gradually heat up to 160-170 C after the addition, keep the reaction 5-6 h, distillation under reduced pressure, portion ethyl acetate was distilled off, the temperature of the solution is reduced to 35--38 C, the reaction solution was pour 500ml sodium bisulfite solution, allowed to stand, aqueous layer was added molecular sieves to decolorize, filtered and the filtrate was added oxalic acid solution, adjusted to pH 3-4, the precipitated solid was recrystallized from ethylene diamine solution, got white solid N-p-hydroxyphenyl salicylamide . |
