化学合成。
有机合成
合成路线 1(1. 合成:3676-85-5)
产率:97%
合成条件:With hydrogen In DMF (N,N-dimethyl-formamide) at 20 - 50℃;
实验步骤:将4-硝基邻苯二甲酰亚胺(LOOGR)加入氢化容器中并使用600ML的二甲基甲酰胺溶解。 将阮内镍催化剂(20gr,湿的)加入到溶液中并在20-30℃和20-40psi压力下开始氢化。 在反应的放热性质结束后,氢气压力增加到40-60psi,温度增加到40-50℃。 氢化结束后,将反应混合物趁热过滤,过滤除去催化剂。 在60-80℃减压下从滤液中除去二甲基甲酰胺。 将水(500ML)加入到残余物中,并将混合物搅拌20-30MIN。 通过过滤分离产物,并在60-70℃下干燥,得到4-氨基邻苯二甲酰亚胺的黄色结晶固体(82gr,97%)。 熔点:293-5℃。
参考文献:
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