反应详情

温度

70 °C

Aqueous ammonia solution (2.5 mL, 30%) was added to a solution of Example 56k (0.4 g, 0.93 mmol) in methanol (1 mL). The reaction mixture was sealed under argon in a reactor vessel and kept in an oven at 120° C. for 2 h. It was concentrated and the solid obtained was washed thoroughly with methanol to remove excess ammonia and dried under vacuo. It was treated with a methanolic HCl solution and stirred at 70° C. for 3 h. The reaction mixture was concentrated, treated with 10% aqueous sodium bicarbonate solution and extracted with ethylacetate. The organic layer was washed with water, brine, dried, and purified using flash chromatography (silica gel, 10% methanol/chloroform) to obtain the title compound as a white solid. Yield: 0.340 g, (89.23%); 1H NMR (DMSO-d6): δ 2.70 (s, 3H, CH3), 3.00 (t, 2H, CH2), 3.35 (t, 2H, CH2), 3.90 (s, 3H, OCH3), 5.20 (s, 2H, CH2), 6.40 (t, 1H, NH), 6.80 (s, 2H, Ar), 7.80 (t, 2H, NH2), 8.15 (s, 1H, Ar) and 8.30 (s, 1H, Ar). MS: m/e (CI+) 411 (M+).

1. customThe reaction mixture was sealed under argon in a reactor vessel
2. concentrationIt was concentrated
3. customthe solid obtained
4. washwas washed thoroughly with methanol
5. customto remove excess ammonia
6. customdried under vacuo
7. additionIt was treated with a methanolic HCl solution
8. concentrationThe reaction mixture was concentrated
9. additiontreated with 10% aqueous sodium bicarbonate solution
10. extractionextracted with ethylacetate
11. washThe organic layer was washed with water, brine
12. customdried
13. custompurified