反应详情

To a solution of cis-1-(4-hydroxy-cyclohexyl)-pyrrolidin-2-one in CH2Cl2 at −30° C., add 786 mL of DAST dropwise. Allow the resulting mixture to warm up to room temp and let 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) and then dry the organic layer over Na2SO4, filter and concentrate. Purify the crude material by chromatography to yield 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