| 摘要 |
Clofibrate drug intermediates chlorophenoxy isobutyrate synthesis method, comprising the following steps: equipped with a stirrer, a thermometer, reflux condenser, a dropping funnel, the reaction vessel was added 0.62mol chlorophenoxy amine solution(2), 300ml hexane solution, 500ml sodium sulfite solution, 0.71-0.73mol acetamide solution(3), controlling the stirring speed at 130-160rpm, the solution temperature was raised to 60-650 C, 0.75-0.79mol 1-bromo-diamine solution(4), after the addition, maintaining the reflux for 90-130min, adding oxalic acid solution, the pH was adjusted to 4-5, the temperature of the solution is reduced to 3-7 C, the precipitated solid was filtered, washed with salt solution, washed with propionitrile solution, washed with ethylenediamine solution, dehydrated with dehydrating agent, recrystallized from nitromethane solution, got crystals of chlorophenoxy isobutyrate. |
