反应详情

温度

5 °C

To 60 ml of dry DMF in a 250 ml-flask, equipped with a CaCl2-tube, cooled in an ice bath, 29.1 (310 mmol) of OPCl3 is dropwise added and the mixture is stirred for two h at 5° C. Then, 58.5 g (288 mmol) of 16, dissolved in 30 ml of dry DMF, is added and the reaction mixture is stirred for 3 h at 90° C. After cooling down, the mixture is poured into iced water, stirred for 30 min and extracted with dichloromethane. The organic layer is washed with a saturated NaHCO3-solution, with brine and dried over MgSO4. After evaporation of the solvent, the compound is purified with column chromatography (silicagel; eluent:dichloromethane/acetonitrile (90:10 v/v)) and collected as an oil.

1. temperaturecooled in an ice bath
2. additionis added
3. stirringthe reaction mixture is stirred for 3 h at 90° C
4. temperatureAfter cooling down
5. stirringstirred for 30 min
6. extractionextracted with dichloromethane
7. washThe organic layer is washed with a saturated NaHCO3-solution, with brine
8. dry with materialdried over MgSO4
9. customAfter evaporation of the solvent
10. customthe compound is purified with column chromatography (silicagel; eluent:dichloromethane/acetonitrile (90:10 v/v))
11. customcollected as an oil