| 摘要 |
Carbenicillin drug intermediates phenyl malonic acid benzyl ester synthesis method, comprising the following steps: equipped with a stirrer, a thermometer, a reaction vessel was added 0.17-0.19mol phenyl-malonic acid solution, 100ml toluene solution, 0.18 mol N- (3- hydroxyphenyl) acetamide was slowly added, controlling the temperature of the solution at 80-85 C , the reaction time is controlled within 4-5h, vacuum distillation, toluene was distilled off, the residue was added 100ml ethylenediamine solution, 0.16-0.17 mol phenol, was heated under reflux for 3-3.5h, the temperature of the solution is reduced to 40-- 45 C, washed with 50ml saline solution, then extracted with potassium hydroxide solution and controlling pH of solution was at 8-9, the extracts were combined, washed with 200ml toluene solution, the aqueous layer was washed with potassium bicarbonate solution, the resulting oil was extracted with methylamine thoroughly, extracted methylamine layer was washed with water, dehydrated with dehydrating agent, the solvent was distilled off, the resulting solid was recrystallized from isopropanol, ultimately got colorless needlelike phenyl malonic acid benzyl ester. |
