反应详情

温度

70 °C

A 30% methanolic methylamine solution (4 mL) was added to a solution of the carboxylic acid of Example 56k (0.5 g, 1.16 mmol) in methanol, in a pressure reactor vessel under nitrogen atmosphere and kept at 110° C. for 4 h. The reaction mixture was cooled, concentrated partially and the solid that precipitated was filtered, washed with methanol, dried, treated with methanolic HCl solution (10 mL) and stirred at 70° C. for 1.5 h. The reaction mixture was cooled and the solid that precipitated was filtered and washed with methanol to obtain the title compound as an off white solid. Yield: 0.325 g, (65.92%); 1H NMR (DMSO-d6): δ 2.50 (d, 3H, CH3), 2.80 (s, 3H, CH3), 3.10 (t, 2H, CH2), 3.30 (t, 2H, CH2), 3.90 (s, 3H, OCH3), 5.10 (s, 2H, CH2), 6.85-6.90 (m, 2H, Ar), 8.10 (s, 1H, Ar), 8.20 (s, 1H, Ar), 9.0 (t, 1H, NH); MS: m/e (ES+) 425 (M+).

1. temperatureThe reaction mixture was cooled
2. concentrationconcentrated partially
3. customthe solid that precipitated
4. filtrationwas filtered
5. washwashed with methanol
6. customdried
7. additiontreated with methanolic HCl solution (10 mL)
8. temperatureThe reaction mixture was cooled
9. customthe solid that precipitated
10. filtrationwas filtered
11. washwashed with methanol