| 摘要 |
Itaconic acid drug intermediates 3-carboxy-2-pentene-1,5-diacid synthesis method, comprising the following steps: equipped with a stirrer, a thermometer, a dropping funnel, the reaction vessel was added 310ml cyclohexane solution, 1.3mol 2-bromo-nitrobenzene solution(3), 1.6-1.9mol 3-amino- 1,3,5-tricarboxylic acid solution(2), 0.56mol cuprous chloride solution, controlling the stirring speed at 150-190rpm, the temperature of solution was raised to 110-115'C, reacted for 3-5h, the temperature of the solution was reduced to 60-65 C, controlling the stirring speed at 200-230rpm, the reaction was continued for 90-120min, the precipitated solid was suction filtered, the solid was added to 200ml oxalic acid solution, stirred for 30-50min, suction filtered, washed with ethyl acetate solution, dehydrated with dehydrating agent, recrystallized from nitromethane solution, got crystals of 3-carboxy-2-pentene-1,5-diacid. |
