反应详情

Methanesulfonyl chloride (0.15 mL, 1.94 mmol) was slowly added to an ice-cooled solution of (4-amino-phenyl)-(4-methoxy-phenyl)-methanone (178) (0.4 g, 1.76 mmol) and pyridine (0.16 mL, 1.94 mmol) in dry dichloromethane (5 mL). The reaction mixture was stirred at room temperature for 20 h then diluted with EtOAc and water. The layers were separated and the aqueous layer was extracted with EtOAc. The organic extracts were combined, washed with brine, dried over Na2SO4, filtered and concentrated to give 0.5 g (93%) of compound 179 as a solid. 1H NMR (400 MHz, DMSO-d6): δ 3.11 (s, 3 H), 3.84 (s, 3 H), 7.06 (d, J=8.8 Hz, 2 H), 7.30 (d, J=8.6 Hz, 2 H), 7.68-7.72 (m, 4 H), 10.31 (s, 1 H).

1. customThe layers were separated
2. extractionthe aqueous layer was extracted with EtOAc
3. washwashed with brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated