Ammonium Chloride → 1-(1-Phenylcyclopropyl)ethan-1-one

HRID 1166611노트

반응식

HRID 1166611 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]=1

참가 물질

5

반응물 3

HCID 25517Ammonium ChlorideHCID 18000813HCID 18000813, 화합물HCID 178418348HCID 178418348, 화합물

생성물 1

HCID 122572631-(1-Phenylcyclopropyl)ethan-1-one

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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

  1. extractionAfter extraction with ethyl acetate
  2. customthe organic phase is dried on sodium sulfate
  3. concentrationconcentrated by evaporation
  4. customThe residue is chromatographed on silica gel with ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-0ab13ffa5f604d4db40a866c0f150629
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06613920B1

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