反应详情

温度

0 °C

Triethylamine (1.16 mL, 8.61 mmol) was added to a stirred solution of compound of Example 37a (2.87 g, 11.78 mmol) and compound of Example 1f (1.5 g, 5.74 mmol) in dry dichloromethane (75 mL). The reaction mixture was stirred at 0° C. for 20 min, was poured in water (100 mL) and extracted with chloroform (2×50 mL). The combined extract was washed with water (50 mL), brine (50 mL) and concentrated under vacuum to obtain the crude product, which was purified by column chromatography (silica gel, 5% ethyl acetate in pet ether 60-80° C.) to obtain the title compound. Yield: 1.93 g, (77.82%); 1H NMR (DMSO-d6, 300 MHz): δ 2.55 (s, 3H, CH3), 3.90 (s, 3H, OCH3), 4.25 (s, 2H, CH2), 7.45 (s, 1H, Ar), 7.50-7.60 (m, 2H, Ar), 7.75 (s, 1H, Ar), 7.85 (s, 1H, Ar); MS: m/e (ES−) 431 (M−1).

1. extractionextracted with chloroform (2×50 mL)
2. extractionThe combined extract
3. washwas washed with water (50 mL), brine (50 mL)
4. concentrationconcentrated under vacuum
5. customto obtain the crude product, which
6. customwas purified by column chromatography (silica gel, 5% ethyl acetate in pet ether 60-80° C.)