反应详情

To a solution of 4-fluoro-2-(morpholinosulfonyl)phenol (0.4 g, 1.5 mmol) and DMAP (0.28 g 2.29 mmol) in CH2Cl2(10 ml), Tf2O (0.93 ml 5.5 mmol) was added dropwise at 0° C. The mixture was stirred at room temperature for 4 h, after which the mixture was washed with hydrochloric acid (1N, 20 ml) and then extracted with EA. The extracts were combined, washed with brine, dried over sodium sulfate and evaporated into dryness. The resulting residue was purified by column chromatography using PE/EA (10/1) as eluent to give the desired product (469 mg, yield 78%).

1. washafter which the mixture was washed with hydrochloric acid (1N, 20 ml)
2. extractionextracted with EA
3. washwashed with brine
4. dry with materialdried over sodium sulfate
5. customevaporated into dryness
6. customThe resulting residue was purified by column chromatography