反应详情

温度

100 °C

Pyrrolidine (0.14 mL, 1.74 mmol) was added to a solution of Example 56k (0.5 g, 1.16 mmol) in dry DMF (5 mL) in an atmosphere of nitrogen. It was stirred at 100° C. for 5 h. The reaction mixture was concentrated and treated with chilled water to obtain a solid which was filtered, washed with water, dried and purified using flash chromatography (silica gel, 2% methanol/chloroform) to obtain the title compound. Yield: 0.375 g, (69.44%); 1H NMR (DMSO-d6): δ 1.75 (m, 4H, 2CH2), 2.70 (s, 3H, CH3), 2.85 (m, 2H, CH2), 3.20 (m, 2H, CH2), 3.90 (s, 3H, OCH3), 5.20 (s, 2H, CH2), 6.25 (t, 1H, NH), 6.7 (s, 2H, 2Ar), 8.20 (s, 1H, Ar), 8.25 (s, 1H, Ar); MS: m/e (ES−) 463 (M+).

1. concentrationThe reaction mixture was concentrated
2. additiontreated with chilled water
3. customto obtain a solid which
4. filtrationwas filtered
5. washwashed with water
6. customdried
7. custompurified