反应详情

To a solution of 3-bromo-5-fluoroaniline (CAS 134168-97-1) (1.0 g, 5.3 mmol) and 2,6-lutidine (2.8 g, 26.5 mmol) in anhydrous DCM (30 mL), was added dropwise 2-chloro-ethanesulfonyl chloride (CAS 1622-32-8) (1.0 g, 6.3 mmol) in DCM (5 mL) at r.t. The mixture was stirred at r.t. for 30 min, and compound 34-A (1.5 g, 16 mmol) was added and stirred for 1 h. Water (50 mL) was added, and the mixture was extracted with EtOAc (100 mL×2). The combined organic layers was washed with sat NaCl (50 mL), dried over Na2SO4, concentrated, and purified by column to give the product (700 mg, yield 37%).

1. stirringstirred for 1 h
2. extractionthe mixture was extracted with EtOAc (100 mL×2)
3. washThe combined organic layers was washed with sat NaCl (50 mL)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. custompurified by column