反应详情

The product from Example 277B (1.00 g, 2.87 mmol) in pyridine (5 mL) was treated with methanesulfonyl chloride (5.56 μL, 7.17 mmol). After stirring for 30 minutes, the mixture was concentrated under reduced pressure and diluted with CH2Cl2 (50 mL). The organic layer was washed with water (50 mL×3), dried (Na2SO4), filtered, and the filtrate concentrated under reduce pressure to provide the title compound. MS (ESI+) m/z 427 (M+H)+; MS (ESI−) m/z 425 (M−H)−; 1H NMR (DMSO, 300 MHz) δ 1.27 (s, 9H), 2.37 (s, 3H), 4.27 (dq, J1 14.9, J2 6.1, 2H), 6.84 (s, 1H), 7.17 (d, J 8.5, 2H), 7.38 (d, J 8.5, 2H), 8.07 (m, 2H), 8.37 (d, J 8.1, 1H), 8.60 (d, J 6.1, 1H), 8.97 (m, 1H), 9.21 (t, J 6.1, 1H), 9.96 (s, 1H).

1. concentrationthe mixture was concentrated under reduced pressure
2. additiondiluted with CH2Cl2 (50 mL)
3. washThe organic layer was washed with water (50 mL×3)
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationthe filtrate concentrated