反应详情

A mixture of 3-bromo-4-(4-chlorophenoxy)-benzoic acid (Preparation 29, 19 g, 58 mmol), methanesulfonamide (9.67 g, 102 mmol), EDCI (19.33 g, 101.5 mmol) and DMAP (12.34 g, 101.5 mmol) in DMF (200 mL) was stirred at room temperature for 16 hours. The reaction mixture was evaporated in vacuo, diluted with DCM (500 mL), washed with aqueous 1M HCl (3×100 mL), dried over sodium sulfate, filtered and concentrated in vacuo. The residue was purified by silica gel chromatography eluting with 50% petroleum ether in EtOAc to afford the title compound as a white solid (5.4 g).

1. customThe reaction mixture was evaporated in vacuo
2. additiondiluted with DCM (500 mL)
3. washwashed with aqueous 1M HCl (3×100 mL)
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified by silica gel chromatography
8. washeluting with 50% petroleum ether in EtOAc