3-氨基-4-羟基苯甲酸的合成The Synthesis of 3-Amino-4-hydroxybenzoic Acid
倪生良,骆浩敏,沈荣明,向长胜
摘要(Abstract):
从3硝基4氯苯甲酸,通过碱性水解、催化加氢及脱盐三步反应,合成得到3氨基4羟基苯甲酸.结果表明,最佳NaOH水解量为5.05.5eq,时间为3.5h;正交试验催化加氢较佳条件为:H2压力为0.25Mpa,pH在5.45.5eq,时间为3.5h;正交试验催化加氢较佳条件为:H2压力为0.25Mpa,pH在5.45.6,反应温度为100℃,催化剂5%Pd C的用量为2.5%(3硝基4羟基苯甲酸).氢化后粗品经重结晶得白色结晶体3氨基4羟基苯甲酸盐酸盐,调pH至2,得3氨基4羟基苯甲酸,纯度(HPLC)≥99.5%,反应总得率为84.3%.
关键词(KeyWords): 3-氨基-4-羟基苯甲酸;3-硝基-4-氯苯甲酸;合成
基金项目(Foundation):
作者(Author): 倪生良,骆浩敏,沈荣明,向长胜
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