反应详情

A solution of t-BuCOCl (7.6 g, 0.063 mol) in DCM (150 mL) was slowly added to a solution of N-(3-amino-4-{[(4,4-difluorocyclohexyl)methyl]amino}phenyl)ethanesulfonamide (22 g, 0.063 mol) and Et3N (9.7 mL, 0.069 mol) in DCM (500 mL) at 0° C. The reaction mixture was stirred for 3 hrs. at 0° C. DCM (300 mL) and water (200 mL) were added. The organic layer was separated and washed with water (3×200 mL), brine and dried over anhydrous Na2SO4. The solvent was removed and the crude product was purified on silica gel by flash chromatography (EtOAc:hexane 1:1) to provide the title product (23.3 g) as beige solid.

1. customat 0° C
2. customThe organic layer was separated
3. washwashed with water (3×200 mL), brine
4. dry with materialdried over anhydrous Na2SO4
5. customThe solvent was removed
6. customthe crude product was purified on silica gel by flash chromatography (EtOAc:hexane 1:1)