反应详情

温度

80 °C

Methoxy-acetyl chloride (0.6 mL, 6.4 mmol) was added to a solution of Example 72k (0.3 g, 0.64 mmol) with stirring. The temperature was raised to 80° C. and stirring continued for 2 h. The reaction mixture was treated with methanol (1 mL), water and extracted with chloroform. The organic layer was washed with water, brine, dried and purified using flash chromatography (silica gel, methanol/chloroform) to obtain the title compound as a white solid. Yield: 0.260 g (75.14%); 1H NMR (DMSO-d6): δ 0.71 (bs, 4H, 2CH2), 2.60 (bs, 4H, 2CH2), 2.70 (s, 3H, CH3), 3.20 (s, 3H, OCH3), 3.70 (s, 3H, CH3), 3.80 (bs, 4H, 2CH2), 4.00 (s, 3H, OCH3), 5.40 (s, 2H, CH2), 7.65 (s, 1H, Ar), 7.80 (s, 1H, Ar), 8.19 (s, 1H, Ar). 8.22 (s, 1H, Ar); MS: m/e (CI+) 533 (M+1).

1. stirringstirring
2. extractionextracted with chloroform
3. washThe organic layer was washed with water, brine
4. customdried
5. custompurified