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
To a solution of (6R,7R)-4-(tert-butoxycarbonyl)-7-(3,4-dichlorophenyl)-1,4-oxazepane-6-carboxylic acid (590 mg) in acetonitrile (15.1 mL) were added N,N-dimethyl-4-aminopyridine (203 mg), methanesulfonamide (158 mg) and 2-methyl-6-nitrobenzoic anhydride (625 mg) at room temperature, and the mixture was stirred at room temperature for 2 hr. To the reaction mixture was added aqueous ammonium chloride solution, and the mixture was extracted with ethyl acetate. The extract was washed with distilled water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel chromatography (hexane/ethyl acetate) to give the title compound (323 mg).
WORKUP
后处理
- extractionthe mixture was extracted with ethyl acetate
- washThe extract was washed with distilled water and brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated under reduced pressure
- customthe residue was purified by silica gel chromatography (hexane/ethyl acetate)