HRID644428
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
PROCEDURE
实验过程
A mixture of N-[3,5-bis(trifluoromethyl)phenyl]-2-methoxy-5-sulfamoyl-benzamide (compound of Example 87(2); 442 mg, 1 mmol), 2,5-dimethoxytetrahydrofuran (159 mg, 1.2 mmol) and acetic acid (5 mL) was refluxed for 2 hours. After cooling, the reaction mixture was poured into water and extracted with ethyl acetate. After the organic layer was washed with water, saturated aqueous sodium hydrogen carbonate and brine, dried over anhydrous magnesium sulfate, the residue obtained by evaporation of the solvent under reduced pressure was purified by chromatography on silica gel (n-hexane:ethyl acetate=3:2) to give the title compound (436.5 mg, 88.6%) as a white solid.
WORKUP
后处理
- temperaturewas refluxed for 2 hours
- temperatureAfter cooling
- extractionextracted with ethyl acetate
- washAfter the organic layer was washed with water, saturated aqueous sodium hydrogen carbonate and brine
- dry with materialdried over anhydrous magnesium sulfate
- customthe residue obtained by evaporation of the solvent under reduced pressure
- customwas purified by chromatography on silica gel (n-hexane:ethyl acetate=3:2)