反应详情

A mixture of Example 133 (0.4 g, 0.9 mmol), dimethylamine.HCl (0.44 g, 5.4 mmol) and potassium carbonate (0.75 g, 5.0 mmol) in 10 mL of dry DMF was stirred at 80° C. for 2 h. The reaction mixture was filtered and the solid obtained was washed with water. The filtrate was concentrated, treated with water and extracted with chloroform. The organic layer was washed with water, brine, concentrated and purified using flash chromatography (silica gel, 1% methanol/chloroform) to obtain the title compound. Yield: 0.26 g, (63.73%); 1H NMR (DMSO-d6): δ 1.96 (s, 6H, 2CH3), 2.17 (s, 2H, CH2), 2.3 (s, 3H, CH3), 3.51 (s, 3H, OCH3), 4.45 (s, 2H, CH2), 7.29 (s, 1H, Ar), 7.55 (s, 1H, Ar), 7.67 (s, 1H, Ar), 7.95 (s, 1H, Ar), 9.26 (s, 1H, NH); MS: m/e (EI+) 451 (M+1).

1. filtrationThe reaction mixture was filtered
2. customthe solid obtained
3. washwas washed with water
4. concentrationThe filtrate was concentrated
5. additiontreated with water
6. extractionextracted with chloroform
7. washThe organic layer was washed with water, brine
8. concentrationconcentrated
9. custompurified