HRID2283301
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 2-amino-5-methyl-benzenesulfonamide (1.86 g, 1 mmol) in pyridine (20 mL), 2,3-dichlorobenzenesulphonyl chloride (3.0 g, 1.25 mmol) was added at 0° C. The reaction was stirred at RT for 17 h. The pyridine was removed in vacuo and the residue was dissolved in ethyl acetate. The organic phase was washed with aqueous 1N HCl, water and brine, dried over sodium sulfate, and concentrated under reduced pressure. The crude product was purified by flash column chromatography using ethyl acetate/hexane (1:1) as eluent to give the title compound (2.4 g, 60%).
WORKUP
后处理
- customThe pyridine was removed in vacuo
- dissolutionthe residue was dissolved in ethyl acetate
- washThe organic phase was washed with aqueous 1N HCl, water and brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe crude product was purified by flash column chromatography