HRID918604
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 4-chloro-3-nitro-5-chlorosulphonyl-benzoic acid (6 g) in ethyl acetate (50 ml), aniline (7.5 g) was added, while stirring. The reaction mixture was stirred for a further 8 hours and filtered. The filtrate was evaporated, and the residue was dissolved in a mixture of aqueous sodium hydrogen carbonate and diethyl ether. The aqueous layer was separated, and the 4-anilino-3-nitro-5-phenylsulphamyl-benzoic acid was precipitated by addition of 4N hydrochloric acid. After recrystallization from aqueous ethanol (25% ethanol in water), the melting point was 249°-250°C.
WORKUP
后处理
- stirringThe reaction mixture was stirred for a further 8 hours
- filtrationfiltered
- customThe filtrate was evaporated
- dissolutionthe residue was dissolved in a mixture of aqueous sodium hydrogen carbonate and diethyl ether
- customThe aqueous layer was separated
- customthe 4-anilino-3-nitro-5-phenylsulphamyl-benzoic acid was precipitated by addition of 4N hydrochloric acid
- customAfter recrystallization from aqueous ethanol (25% ethanol in water)