반응식
S(Cl)([Cl:4])(=O)=O.[C:6]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])(=[O:10])[CH:7]([CH3:9])[CH3:8].O.C([O-])(O)=O.[Na+].[C:23]1([CH3:29])C=CC=C[CH:24]=1>>[Cl:4][CH:11]([C:6](=[O:10])[C:7]1[CH:9]=[CH:29][CH:23]=[CH:24][CH:8]=1)[C:12]([O:14][CH2:15][CH3:16])=[O:13]참가 물질
6
실험 절차
A solution of sulfuryl chloride (12.4 mmol) in toluene (5 mL) was added dropwise via an additional funnel to a solution of ethyl isobutyrylacetate (12.4 mmol) in toluene (20 mL) over 5 minutes at room temperature. The resulting mixture was stirred at room temperature overnight. Water was added slowly and resulting two-phase mixture was basified with saturated NaHCO3 and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over anhydrous sodium sulfate, and evaporated to afford 2.2 g (84%) of product as a pale yellow oil: MH+=227.0, retention time (LC-MS)=2.77 min.
후처리
- customresulting two-phase mixture
- extractionextracted with ethyl acetate
- washThe combined organic extracts were washed with brine
- dry with materialdried over anhydrous sodium sulfate
- customevaporated
출처 및 근거
- ORD 기록
- ord-d5f1d0d3073d452b8ad7c8c476d8d731
- 출처 데이터셋
- uspto-grants-2004_03
- 특허 번호
- US06699860B2
연결된 노트
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