奥沙拉嗪合成工艺的改进

An Improved Synthetic Process of Osalazine

将9·1g亚硝酸钠在15℃以下滴加到15·3g5-氨基水杨酸(5-ASA)和30mL盐酸组成的混合液中,重氮化反应2h制得中间体5-ASA重氮盐(氯化偶氮水杨酸);然后与0·2mol水杨酸钠在碱性条件下偶合,得到粗品。用水重结晶,得到棕黄色粉状结晶奥沙拉嗪21·2g,即3,3’-偶氮(6-羟基苯甲酸)二钠盐,以5-ASA计收率为61·2%。

9.1 g Sodium nitrite was added dropwise to a mixture composed of 15.3g 5-aminosalicylic acid （5-ASA）and 30mL hydrochloric acid at temperature below 15℃. After diazotization for 2 hours the intermediate diazonium salt （chlorinated azosalicylic acid） was formed l which was coupled with 0. 2tool sodium salicylate under alkaline condition. The crude product was obtained after recrystallization was carried out in water, and 21.2g brown yellow powder of Osalazine, named 3,3＇-azobis（6-hydroxybenzoic acid）disodium with 95% purity was given. The total yield was 61.2% （calculated based on 5-aminosalicylic acid）.