反应详情

To a solution of trans-1-(4-hydroxy-cyclohexyl)-pyrrolidin-2-one (3.2 g) in CH2Cl2 (10 mL) at −30° C., add 2.75 mL of DAST dropwise. Allow the resulting mixture to warm up to room temp and stand for 1 h. To the solution, add 10 mL of 5% aq NaHCO3 and allow to stand at room temp for 1 h. Extract the aqueous layer by CH2Cl2 twice (2×10 mL). Dry the organic layer over Na2SO4, filter and concentrate. Purify the crude material by chromatography to yield 2.05 g of the title compound: mass spectrum (m/z): 186 (M+1).

1. waitto stand at room temp for 1 h
2. extractionExtract the aqueous layer by CH2Cl2 twice (2×10 mL)
3. dry with materialDry the organic layer over Na2SO4
4. filtrationfilter
5. concentrationconcentrate
6. customPurify the crude material by chromatography