反应详情

温度

0 °C

Amine 5 (4.22 g, 7.9 mmol) is dissolved in anhydrous dichloromethane (25 mL) and cooled to 0° C. To the solution are added pyridine (10 mL) and compound 89 (9.3 g, 7.9 mmol) successively. The reaction temperature was brought to ambient temperature and stirred further. The completion of the reaction is ascertained by TLC (EtOAc). The reaction mixture is diluted with dichloromethane and washed with saturated NaHCO3, water followed by brine. The organic layer is dried over sodium sulfate, filtered and concentrated under vacuum to afford the crude product. Compound 90 is obtained as a white solid after column chromatography over silica gel.

1. customwas brought to ambient temperature
2. washwashed with saturated NaHCO3, water
3. dry with materialThe organic layer is dried over sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated under vacuum
6. customto afford the crude product