反应详情

温度

110 °C

2-piperazin-1-yl-ethanol (0.227 g, 1.74 mmol) was added with stirring to a solution of Example 56k (0.5 g, 1.16 mmol) in DMF (10 mL) in an atmosphere of nitrogen. The reaction mixture was stirred at 110° C. for 6 h, concentrated, treated with chilled water and extracted with n-butanol. 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 an off-white solid. Yield: 0.521 g, (85.69%); 1H NMR (DMSO-d6): δ 2.50 (s, 3H, CH3), 3.10 (t, 4H, 2CH2), 3.70 (t, 10H, 5CH2), 3.90 (s, 3H, OCH3), 4.40 (s, 2H, CH2), 5.20 (s, 2H, CH2), 6.10 (s, 1H, Ar), 6.80-6.85 (m, 2H, Ar), 8.10 (m, 2H, Ar); MS: m/e (ES+) 551 (M+).

1. concentrationconcentrated
2. additiontreated with chilled water
3. extractionextracted with n-butanol
4. washThe organic layer was washed with water, brine
5. customdried
6. concentrationconcentrated
7. custompurified