反应详情

To a solution of 1-(2-bromopyridin-4-yl)-propan-1-ol (2.20 g 10.2 mmol) in dichloromethane (55 mL) is added Dess-Martin periodinane (5.6 g, 13 mmol). After 30 hours, the mixture is diluted with saturated aqueous sodium carbonate (40 mL) and partially concentrated to remove the dichloromethane. The crude material is filtered through filter agent and washed with EtOAc (100 mL). The aqueous layer is separated and extracted with EtOAc (40 mL). The combined organic layers are washed with saturated aqueous sodium carbonate (40 mL) and brine (40 mL). The material is dried over magnesium sulfate, filtered and concentrated to afford 1-(2-bromopyridin-4-yl)-propan-1-one as an oil which is used without further purification.

1. concentrationpartially concentrated
2. customto remove the dichloromethane
3. filtrationThe crude material is filtered
4. filtrationthrough filter agent
5. washwashed with EtOAc (100 mL)
6. customThe aqueous layer is separated
7. extractionextracted with EtOAc (40 mL)
8. washThe combined organic layers are washed with saturated aqueous sodium carbonate (40 mL) and brine (40 mL)
9. dry with materialThe material is dried over magnesium sulfate
10. filtrationfiltered
11. concentrationconcentrated