反应详情

温度

80 °C

To a solution of tert-butyl(3S)-3-{[6-chloro-2-(methylsulfanyl)-5-{2-[(methylsulfonyl)oxy]ethyl}pyrimidin-4-yl]amino}-3-methylpyrrolidine-1-carboxylate (1635 mg, 3.4 mmol) in DMF (34 mL) was added DBU (1.1 mL, 6.8 mmol) and the mixture was stirred at 80° C. for 90 min. The reaction mixture was diluted with EtOAc (20 mL), washed with water (20 mL) and brine (20 mL), dried over Na2SO4 and concentrated to give the title compound (1.24 g, 95%) as a light yellow-white solid. 1H NMR (400 MHz, DMSO-d6) δ 3.80-3.57 (m, 4 H), 3.40-3.35 (m, 1 H), 3.28-3.19 (m, 1 H), 2.91 (t, J=8.9 Hz, 2 H), 2.42 (s, 3 H), 2.39-2.24 (m, 1 H), 2.07-1.94 (m, 1 H), 1.39 (d, J=5.4 Hz, 9 H), 1.28 (s, 3 H). m/z (APCI+) for C17H25ClN4O2S 385.1 (M+H)+.

1. washwashed with water (20 mL) and brine (20 mL)
2. dry with materialdried over Na2SO4
3. concentrationconcentrated