反应详情

A solution of 3,5-dichloro-4-(6-chloro-benzothiazol-2-yloxy)phenylamine (364) (2.0 g, 5.79 mmol) and 3-chloro-4-trifluoromethylbenzenesulfonylchloride (1.7 g, 6.08 mmol) in pyridine (10 ml) was stirred at room temperature. After 3-hr water was added to the reaction mixture, which was then acidify by 2N HCl. Reaction mixture was extracted twice with AcOEt. Organic layer was washed by brine, dried over MgSO4 and concentrated. Crude residue was purified by column chromatography (H/A=4/1, 80 g of silica gel) to afford title compound 365 (2.11 g, 65%) as a white solid. mp 82–84° C.

1. customReaction mixture
2. extractionwas extracted twice with AcOEt
3. washOrganic layer was washed by brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customCrude residue was purified by column chromatography (H/A=4/1, 80 g of silica gel)