反应详情

温度

10 °C

Tetrahydro-pyran-4-ol (1.01 g, 5.01 mmol) was added dropwise at 0° C. to a suspension of sodium hydride (200 mg, 5.01 mmol) in DMSO (10 ml). After stirring for 30 min at 10° C., a solution of the product obtained from step 1 (850 mg, 3.34 mmol) in DMSO (2 ml) was added dropwise and stirring was continued for 1 h at RT. The reaction was quenched with ice/water (50 ml). Ethyl acetate (50 ml) was added and the aqueous phase was extrated with ethyl acetate (2×30 ml). The combined organic phases were washed with brine (2×50 ml), dried over sodium sulphate, filtered, and evaporated. The product was obtained in quantitative yield and used in the next step without further purification.

1. stirringstirring
2. waitwas continued for 1 h at RT
3. customThe reaction was quenched with ice/water (50 ml)
4. additionEthyl acetate (50 ml) was added
5. washThe combined organic phases were washed with brine (2×50 ml)
6. dry with materialdried over sodium sulphate
7. filtrationfiltered
8. customevaporated
9. customThe product was obtained in quantitative yield
10. customused in the next step without further purification