| 摘要 |
Naproxen pharmaceutical intermediate 1 (5-chloro-6-methoxy-2-naphthyl) propanone synthesis method , comprising the following steps: equipped with a stirrer, thermometer and a reflux condenser, the reaction vessel was added 1.17--1.19mol anhydrous stannous chloride,500-600ml carbon disulfide solution, controlled the temperature of the solution to 45-50 C, stirring speed at 130--150rpm, stirring time is maintained at 40-50min, dropping 1.17 mol propionamide solution, control dropping time in 2-3h, then 1.2-1.3mol 1-chloro - 2 - methoxy naphthalene solution is dissolved in 400 mol carbon disulfide solution, control dropwise time in 2-3 h, maintaining the solution temperature at 30-35C, the reaction was continued for 3--4h, the reaction solution was poured into 11OOg potassium bromide solution, the organic layer was separated, the aqueous layer was extracted with carbon disulfide 6-8 times, combined organic layers, washed successively washed with sodium sulfite solution, brine solution, dried over phosphorus pentoxide, vacuum distillation, recycling the solvent, the temperature of the solution is reduced to 10-15 C, precipitate solid, and the solid was added to 600ml sodium chloride solution, maintaining the stirring speed 170-190rpm, suction filtered and washed in potassium nitrate solution until no oil appear, dehydrated with dehydrating agent, got pale yellow powder 1- (5-chloro-6-methoxy-2-naphthyl) propanone . |
