反应详情

温度

0 °C

Isobutylchloroformate (0.17 mL, 1.33 mmol) was added to a solution of Example 72k (0.40 g, 0.88 mmol) in dry CH2Cl2 (15 mL). Triethylamine (0.23 ml, 1.67 mmol) was added and the reaction mixture was stirred at 0° C. for 1 h. It was brought to room temperature, treated with water and extracted with chloroform. The organic layer was washed with water, brine, dried, concentrated and crystallised using ethyl acetate to obtain the title compound as a white solid. Yield: 0.280 g, (58%). 1H NMR (DMSO-d6): δ 0.80 (d, 6H, 2CH3), 1.70-1.80 (m, 5H, 2CH2, CH), 2.50-2.89 (m, 1H, 4CH2, CH3), 3.90 (d, 2H, CH2), 5.19 (s, 2H, CH2), 7.55 (s, 1H, Ar), 7.75 (s, 1H, Ar), 8.10 (s, 1H, Ar), 8.20 (s, 1H, Ar). MS: m/e (EI+) 565 (M+).

1. customwas brought to room temperature
2. extractionextracted with chloroform
3. washThe organic layer was washed with water, brine
4. customdried
5. concentrationconcentrated
6. customcrystallised