反应详情

To a stirring solution of Example 158 (0.400 g, 0.914 mmol) and pyridine (0.591 mL, 7.312 mmol) in dichloromethane was added methanesulfonyl chloride (0.141 mL, 1.829 mmol) dropwise over 5 minutes and the resulting reaction mixture stirred for 12 hours. The solution was concentrated in. vacuo and purified by flash chromatography on SiO2 eluting with a 0-100% ethyl acetate/hexane gradient yielding the title compound (0.365 g, 77% yield) as a light yellow solid. 1H NMR (300 MHz, DMSO-d6): δ ppm −0.22 (m, 2 H) 0.24 (m, 2 H) 0.85 (m, 2 H) 1.57 (s, 3 H) 2.14 (m, 1 H) 2.32 (m, 1 H) 3.08 (s, 3 H) 7.56 (m, 4 H) 7.73 (m, 4 H) 8.14 (d, J=8.09 Hz, 1 H) 10.23 (m, 1 H) 13.79 (m, 1 H). MS (ESI+) m/z=416 (M+H)+.

1. customthe resulting reaction mixture
2. concentrationThe solution was concentrated in
3. customvacuo and purified by flash chromatography on SiO2 eluting with a 0-100% ethyl acetate/hexane