반응식
[C:1]([Si:5]([CH3:12])([CH3:11])[O:6][CH2:7][C:8]([CH3:10])=O)([CH3:4])([CH3:3])[CH3:2].[CH3:13][C:14]([S@@:17]([NH2:19])=[O:18])([CH3:16])[CH3:15].[Cl-].[Na+]>C1COCC1.CCO.CCO.CCO.CCO.[Ti]>[Si:5]([O:6][CH2:7]/[C:8](=[N:19]/[S@:17]([C:14]([CH3:16])([CH3:15])[CH3:13])=[O:18])/[CH3:10])([C:1]([CH3:4])([CH3:3])[CH3:2])([CH3:12])[CH3:11]참가 물질
반응물 3
생성물 1
시약·촉매·용매 2
반응 조건
- 온도
- 70 °C
실험 절차
To a solution of 761 mg of 1-{[tert-butyl (dimethyl)silyl]oxy}acetone in 20 ml of THF were added 2.1 ml of tetraethyl orthotitanate and 490 mg of (S)-2-methylpropane-2-sulfinamide, followed by stirring at 70° C. for 8 hours. The reaction mixture was left to be cooled to room temperature and a saturated aqueous sodium chloride solution was then added thereto, followed by stirring and filtering over Celite. The filtrate was extracted with ethyl acetate. The organic layer was washed with a saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate, and the solvent was then evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain (S)—N-[(2E)-1-{[tert-butyl(dimethyl)silyl]oxy}propan-2-ylidene]-2-methylpropane-2-sulfinamide.
후처리
- waitThe reaction mixture was left
- temperatureto be cooled to room temperature
- stirringby stirring
- filtrationfiltering over Celite
- extractionThe filtrate was extracted with ethyl acetate
- washThe organic layer was washed with a saturated aqueous sodium chloride solution
- dry with materialdried over anhydrous magnesium sulfate
- customthe solvent was then evaporated under reduced pressure
- customThe obtained residue was purified by silica gel column chromatography
출처 및 근거
- ORD 기록
- ord-81a2ccdcebbb4547ac546954f461f188
- 출처 데이터셋
- uspto-grants-2016_03
- 특허 번호
- US09278968B2
연결된 노트
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