| 摘要 |
Carbenicillin sodium amoxicillin drug intermediate benzylidene malonate synthesis method, comprising the following steps: the reaction vessel was added 1.3mol diethyl malonate(3), 1.6-1.9mol benzylamine alcohol solution(2), 500ml cyclohexane, 1.5mol alumina, 200ml toluene, the solution temperature is raised to 80-85C, refluxed for 5-8h, the temperature of the solution is reduced to 60-65C, the reaction was continued 80-110min, the temperature of the solution is reduced to 10-17C, allowed to stand for 2-5h, layers were separated and removed the oil layer, washed with oxalic acid solution, washed potassium sulfite solution, the solution was extracted for 5-7 times with xylene solution, the combined extracts were dehydrated with dehydrating agent, vacuum distillation, collecting fractions of 110-117C, recrystallized in the acetonitrile solution, ultimately got crystals of benzylidene malonate ethyl ester. |
