HRID1846328
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 115 °C
PROCEDURE
实验过程
Isatoic anhydride (0.690 g, 4.20 mmol) was added to a solution of N-(4-aminophenyl)propane-2-sulfonamide (0.910 g, 4.20 mmol) in DMF (15 mL) and heated at 115° C. overnight. The mixture was concentrated in vacuo and purified by flash chromatography on silica gel, eluting with 6% MeOH in CH2Cl2. Further purification was effected by reverse phase chromatography, eluting with 10% to 90% CH3CN in H2O with 0.1% TFA. The desired fractions were collected, basified, and extracted with EtOAc to afford 2-amino-N-(4-(1-methylethylsulfonamido)phenyl)benzamide (0.325 g, 23%).
WORKUP
后处理
- concentrationThe mixture was concentrated in vacuo
- custompurified by flash chromatography on silica gel
- washeluting with 6% MeOH in CH2Cl2
- customFurther purification
- washeluting with 10% to 90% CH3CN in H2O with 0.1% TFA
- customThe desired fractions were collected
- extractionextracted with EtOAc