反应详情

To a suspension of [3-methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-(8-phenyl-5,6,7,8-tetrahydro-pyrido[4,3-d]pyrimidin-2-yl)-amine hydrochloride (65 mg, 0.15 mmol) in methylen chloride (2 mL) was added at room temperature NN,-diisopropyl ethyl amine (28 mg, 0.22 mmol) and after 2 minutes acetyl chloride (12.5 mg, 0.16 mmol). The reaction was stirred at room temperature over night. The solvent was evaporated under reduced pressure and the residue was purified by column chromatography on silica gel using dichloromethane/methanol (19:1 v/v) as eluent to yield the title compound (20 mg, 30%) as a yellow gum. MS ISP (m/e): 455.3 (100) [(M+H)+]. 1H NMR (CDCl3, 300 MHz): δ (ppm)=8.38 (s, 1H), 7.61 (s, 1H), 7.56 (s, 1H), 7.20-7.33 (m, 3H), 7.05-7.08 (m, 3H), 6.81 (s, 1H), 6.79 (d, 1H), 5.18 (d, 1H), 4.46 (d, 1H), 4.21 (t, 1H), 3.90 (m, 2H), 3.46 (s, 3H), 2.27 (s, 3H), 1.71 (s, 3H).

1. additionwas added at room temperature NN
2. customThe solvent was evaporated under reduced pressure
3. customthe residue was purified by column chromatography on silica gel