摘要 |
Isoxazole hydrochloride-octyl drug intermediates O-benzoyl benzoic acid synthesis method comprises the following steps: equipped with a stirrer, thermometer and reflux condenser, the reaction vessel was added 0.88mol 2-carboxy - benzyl alcohol solution (2), 700-800ml phenol solution, controlling the stirring speed 130-170rpm, In batches to join 1.9 mol cuprous chloride, after the addition the solution temperature rises to 80 - 85 C, control the reaction time is 5-6 h, the temperature of the solution is reduced to 35 --- 40 C, the reaction solution was poured into 1.3L phosphoric acid solution, the solution temperature is reduced 5--7 C, control the stirring speed 190-230rpm, the precipitated white solid was suction filtered and washed by potassium bromide solution, the filtrate was dissolved in sodium sulfite solution, molecular sieves decolorization, oxalic acid solution was added until the pH value was 3- 4, solid precipitation, the temperature of the solution is reduced to 5 - 7 C, filtered, washed with saline solution, dried at temperature of 75 - 80 C , got O-benzoyl benzoic acid. |