反应详情

温度

110 °C

1-Methyl-piperazine (0.191 g, 1.91 mol) was added to a solution of Example 56k (0.5 g, 1.16 mmol) in dry DMF (10 mL) and stirred at 110° C. for 2 h. The reaction mixture was treated with water and extracted with ethyl acetate. The organic layer was washed with water, brine, dried, concentrated and purified using flash chromatography (silica gel, methanol/chloroform) to obtain the title compound as a white solid. Yield: 0.350 g, (60.97%); 1H NMR (DMSO-d6): δ 2.2 (s, 3H, CH3), 2.5-2.60 (m, 10H, 5CH2), 2.70 (s, 3H, CH3), 3.10 (d, 2H, CH2), 3.90 (s, 3H, CH3), 5.10 (s, 2H, CH2), 6.7 (s, 2H, Ar), 8.01 (s, 1H, Ar), 8.20 (s, 1H, Ar); MS: m/e (ES+) 495 (M+1).

1. extractionextracted with ethyl acetate
2. washThe organic layer was washed with water, brine
3. customdried
4. concentrationconcentrated
5. custompurified