反应详情

温度

55 °C

Cyclopropanecarbonyl chloride (0.44 mL, 4.8 mmol) was added to a solution of Example 72k (0.3 g, 0.64 mmol) and the reaction mixture was stirred at 55° C. for 2 h. It 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: 0.280 g, (81.63%); 1H NMR (DMSO-d6): δ 0.71 (bs, 2H, CH2), 0.88 (bs, 2H, CH2), 1.87 (bs, 2H, CH2), 2.01 (bs, 2H, CH2), 2.70 (s, 3H, CH3), 3.00 (bs, 2H, CH2), 3.18 (bs, 2H, CH2), 3.57 (bs, 2H, CH2), 3.70 (s, 3H, CH3), 3.91 (s, 3H, OCH3), 4.04 (bs, 2H, CH2), 5.38 (s, 2H, CH2), 7.78 (s, 1H, Ar), 7.98 (s, 1H, Ar), 8.19 (s, 1H, Ar), 8.22 (s, 1H, Ar); MS: m/e (CI+) 533 (M+1).

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