反应详情

温度

110 °C

Imidazole (0.118 g, 1.73 mmol) was added in an atmosphere of nitrogen, to a solution of Example 56k (1.3 g, 2.63 mmol) in dry DMF (10 mL) with stirring. The reaction mixture was then maintained at 110° C. for 18 h. It was cooled, concentrated and the solid obtained was filtered washed with water, dried and purified using flash chromatography (silica gel, methanol/chloroform) to obtain the title compound as a white solid. Yield: 0.120 g, (22.38%); 1H NMR (DMSO-d6): δ 2.7 (s, 3H, CH3), 3.2 (t, 2H, CH2), 3.9 (s, 3H, OCH3), 4.1 (t, 2H, CH2), 5.2 (s, 2H, CH2), 6.4 (s, 1H, NH), 6.6 (s, 1H, Ar), 6.75 (s, 1H, Ar), 6.9 (s, 1H, Ar), 7.2 (s, 1H, Ar), 7.6 (s, 1H, Ar), 8.1 (s, 1H, Ar), 8.2 (s, 1H, Ar); MS: m/e (ES+) 462 (M+).

1. temperatureIt was cooled
2. concentrationconcentrated
3. customthe solid obtained
4. filtrationwas filtered
5. washwashed with water
6. customdried
7. custompurified