Ammonium Chloride → 1-(1-Phenylcyclopropyl)ethan-1-one
반응식
CN(C)[C:3]([C:5]1([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:7][CH2:6]1)=[O:4].[CH3:15][Li].[Cl-].[NH4+]>C1COCC1>[C:8]1([C:5]2([C:3](=[O:4])[CH3:15])[CH2:7][CH2:6]2)[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1참가 물질
5
반응 조건
- 온도
- -10 °C
실험 절차
4.34 g of 27 is dissolved in 189 ml of THF, cooled to −10° C., and 21.5 ml of methyllithium solution (1.6 M in diethyl ether) is added in drops under nitrogen. It is stirred for 2 hours at this temperature, and the reaction mixture is then poured into saturated ammonium chloride solution. After extraction with ethyl acetate, the organic phase is dried on sodium sulfate and concentrated by evaporation. The residue is chromatographed on silica gel with ethyl acetate/hexane, whereby 3.7 g of title compound 28 is obtained as a yellowish oil.
후처리
- extractionAfter extraction with ethyl acetate
- customthe organic phase is dried on sodium sulfate
- concentrationconcentrated by evaporation
- customThe residue is chromatographed on silica gel with ethyl acetate/hexane
출처 및 근거
- ORD 기록
- ord-e71d27b923ab460da8e7a56582368f9e
- 출처 데이터셋
- uspto-grants-2003_07
- 특허 번호
- US06600058B1
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