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Diethyl Ether → 6-Ethylthio-3-hepten-2-one

HRID 661772
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HRID 661772 반응식
C1(P(C2C=CC=CC=2)(C2C=CC=CC=2)=[CH:8][C:9](=[O:11])[CH3:10])C=CC=CC=1.[CH2:24]([S:26][CH:27]([CH3:31])[CH2:28][CH:29]=O)[CH3:25].CCCCCC.CCOCC>ClCCl>[CH2:24]([S:26][CH:27]([CH3:31])[CH2:28][CH:29]=[CH:8][C:9](=[O:11])[CH3:10])[CH3:25]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 3283Diethyl EtherHCID 8058HexaneHCID 150381-(Triphenylphosphoranylidene)acetoneHCID 160141Butanal, 3-(ethylthio)-

생성물 1

HCID 544576116-Ethylthio-3-hepten-2-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1-Triphenylphosphoranylidene-2-propanone (12.77 g, 40.0 mmol) is added to a solution of 3-(ethylthio)butyraldehyde (5.30 g, 40.0 mmol) in dichloromethane (100 ml) and the mixture is heated under reflux for 24 hours. The reaction mixture is cooled to room temperature, and the solvent evaporated in vacuo to give a beige solid. The crude product is taken up in a 1:1 mixture of hexane:ether (the insoluble material is discarded), and then concentrated under reduced pressure to give an orange oil which is further purified by column chromatography on silica gel to give 6-(ethylthio)hept-3-en-2-one as a yellow oil.

후처리

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 24 hours
  3. customthe solvent evaporated in vacuo
  4. customto give a beige solid
  5. concentrationthen concentrated under reduced pressure
  6. customto give an orange oil which
  7. customis further purified by column chromatography on silica gel

출처 및 근거

ORD 기록
ord-3c0061b074da4c3bb8dba46c2fd833e8
출처 데이터셋
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08084649B2

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