反应详情

温度

10 °C

7-Cyano-4-chromanol (Step B) (8.0 g, 46 mmol) was dissolved in CH2Cl2 (120 mL) and cooled to 10° C. SOCl2 (5.0 mL, 70 mmol) was added, the reaction was warmed to RT and stirred overnight. The reaction was concentrated in vacuo and azeotroped with CH2Cl2 (2×50 mL). The residue was dissolved in EtOAc (500 mL), washed with saturated NaHCO3 (250 mL), and with brine (150 mL), dried over MgSO4, filtered and concentrated in vacuo to provide the title compound which was used without further purification.

1. temperaturethe reaction was warmed to RT
2. concentrationThe reaction was concentrated in vacuo
3. customazeotroped with CH2Cl2 (2×50 mL)
4. dissolutionThe residue was dissolved in EtOAc (500 mL)
5. washwashed with saturated NaHCO3 (250 mL)
6. dry with materialwith brine (150 mL), dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo