反应详情

温度

70 °C

The product of step d) (200 mg, 0.89 mmol) was dissolved in 15 mL CHCl3 and treated with TMSI (4.5 mmol, 600 uL). After heating to 70° C. overnight, the reaction was carefully quenched with MeOH (10 mL) and 1 M NaOH (20 mL). The subtitle compound was extracted into DCM (3×20 mL). The extracts were dried over MgSO4 and concentrated to give 178 mg of the subtitle compound. 1H NMR (300 MHz, DMSO) 7.20 (d, J=5 Hz, 1H), 6.85 (d, J=5 Hz, 1H), 3.42-3.61 (m, 4H), 2.71-3.03 (m, 4H). MS: ESI (positive): 154 (M+H).

1. customthe reaction was carefully quenched with MeOH (10 mL) and 1 M NaOH (20 mL)
2. extractionThe subtitle compound was extracted into DCM (3×20 mL)
3. dry with materialThe extracts were dried over MgSO4
4. concentrationconcentrated