反应详情

温度

110 °C

Aqueous ammonia solution (30%, 4 mL) was added to a solution of Example 102j (0.5 g, 1.04 mmol) in methanol (1 mL), in an atmosphere of nitrogen, sealed in a pressure reactor vessel and heated at 110° C. for 6 h. The reaction mixture was brought to room temperature, concentrated, treated with chilled water and dilute HCl to neutral pH. The solid that precipitated was filtered, washed with water and dried. It was treated with methanolic HCl solution and stirred at 70° C. for 2.5 h. The reaction mixture was cooled and the solid that separated was filtered, washed with methanol, dried and purified using flash chromatography (silica gel, MeOH/CHCl3) to obtain the title compound as an off white solid. Yield: 0.220 g (48.24%); 1H NMR (DMSO-d6): δ 2.30 (m, 4H, 2CH2), 2.70 (s, 3H, CH3), 3.10 (m, 4H, 2CH2), 3.95 (s, 3H, OCH3), 5.10 (s, 2H, CH2), 7.10 (s, 1H, Ar), 7.20 (s, 1H, Ar), 8.05 (s, 1H, Ar) 8.20 (s, 1H, Ar): MS: m/e (ES+) 422 (M+1).

1. customsealed in a pressure reactor vessel
2. customwas brought to room temperature
3. concentrationconcentrated
4. additiontreated with chilled water and dilute HCl to neutral pH
5. customThe solid that precipitated
6. filtrationwas filtered
7. washwashed with water
8. customdried
9. additionIt was treated with methanolic HCl solution
10. temperatureThe reaction mixture was cooled
11. customthe solid that separated
12. filtrationwas filtered
13. washwashed with methanol
14. customdried
15. custompurified