反应详情

2,3-Dihydropyran (25.0 mL, 270 mmol) was added to (2R)-2-(4-chloro-7H-pyrrolo[2,3-d]pyrimidin-7-yl)propan-1-ol (11.00 g, 51.97 mmol) (see Preparation 3) and pyridinium toluene-4-sulphonate (3.92 g, 15.6 mmol) in DCM (150 mL). The reaction mixture was washed with water (200 mL) and the aqueous phase was extracted with DCM (2×150 mL). The combined organic phases were dried over magnesium sulfate and evaporated in vacuo. The crude material was purified by column chromatography on silica gel (gradient of heptane:EtOAc 100:0 to 70:30) to afford the title compound as a yellow oil in 100% yield, 15.65 g.

1. washThe reaction mixture was washed with water (200 mL)
2. extractionthe aqueous phase was extracted with DCM (2×150 mL)
3. dry with materialThe combined organic phases were dried over magnesium sulfate
4. customevaporated in vacuo
5. customThe crude material was purified by column chromatography on silica gel (gradient of heptane:EtOAc 100:0 to 70:30)