反应详情

温度

80 °C

Cyclopropyl amine (0.285 ml, 4.067 mmol) was added to a solution of Example 133 (0.6 g, 1.35 mmol) in DMF (15 mL) and the reaction mixture was stirred at 80° C. for 2 h. It was concentrated, treated with water and the solid that precipitated was filtered, washed with water and purified using flash chromatography (silica gel, 2% methanol/chloroform) to obtain the title compound as a white solid. Yield: 0.58 g (92%); 1H NMR (CDCl3): δ 0.6 (s, 4H, 2CH2), 2.4 (m, 1H, CH), 2.67 (s, 3H, CH3), 3.6 (s, 2H, CH2), 3.9 (s, 3H, OCH3), 4.7 (s, 2H, CH2), 7.6 (s, 1H, Ar), 7.65 (s, 1H, Ar), 8.1 (s, 1H, Ar), 8.45 (s, 1H, Ar), 9.35 (bs, 1H, NH); MS: m/e (ES+) 465 (M+1).

1. concentrationIt was concentrated
2. additiontreated with water
3. customthe solid that precipitated
4. filtrationwas filtered
5. washwashed with water
6. custompurified