(Diethylamino)sulfur trifluoride → HCID 178516221、化合物
反応式
O[C@H:2]1[CH2:7][CH2:6][C@H:5]([N:8]2[CH2:12][CH2:11][CH2:10][C:9]2=[O:13])[CH2:4][CH2:3]1.CCN(S(F)(F)[F:20])CC.C([O-])(O)=O.[Na+]>C(Cl)Cl>[F:20][C@@H:2]1[CH2:7][CH2:6][C@H:5]([N:8]2[CH2:12][CH2:11][CH2:10][C:9]2=[O:13])[CH2:4][CH2:3]1参加物
5
実験手順
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).
後処理
- waitto stand at room temp for 1 h
- extractionExtract the aqueous layer by CH2Cl2 twice (2×10 mL)
- dry with materialDry the organic layer over Na2SO4
- filtrationfilter
- concentrationconcentrate
- customPurify the crude material by chromatography
出典と根拠
- ORDレコード
- ord-58c56d54590f4339944a941869af2faa
- 出典データセット
- uspto-grants-2011_08
- 特許番号
- US07998999B2
反応ノート
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