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Diethyl Ether → HCID 13243717, 화합물

HRID 614119
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HRID 614119 반응식
[C:1]1([CH2:7][CH2:8]Br)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Mg].[CH3:11][C:12]([C:16]1[CH:21]=[C:20]([O:22][CH3:23])[CH:19]=[C:18]([O:24][CH3:25])[CH:17]=1)([CH3:15])[C:13]#N.CC[O:28]CC>>[CH3:15][C:12]([C:16]1[CH:21]=[C:20]([O:22][CH3:23])[CH:19]=[C:18]([O:24][CH3:25])[CH:17]=1)([C:13](=[O:28])[CH2:8][CH2:7][C:1]1[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1)[CH3:11]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 3283Diethyl Ether2회HCID 7666Phenethyl bromideHCID 5462224MagnesiumHCID 97942622-(3,5-dimethoxyphenyl)-2-methylpropanenitrile

생성물 1

HCID 13243717HCID 13243717, 화합물

실험 절차

To a solution of the Grignard reagent prepared from 2-phenylbromoethane (5.5 g.), magnesium (0.8 g.) and dry ether (60 ml.) is added a solution of 2-methyl-2-(3,5-dimethoxyphenyl)propionitrile (2.75 g.) in dry ether (20 ml.). The ether is distilled off and replaced by dry benzene (50 ml.) and the mixture refluxed for 48 hours. It is then decomposed by careful treatment with dilute sulfuric acid and heated on a steam bath for 1 hour. The mixture is then extracted with ether, the extract dried (MgSO4) and concentrated to an oil. Distillation of the oil in vacuo affords 2-methyl-2-(3,5-dimethoxyphenyl)-5-phenyl-3-pentanone; b.p. 168° C./0.2 mm. (Yield: 2.32 g., 60%)

후처리

  1. distillationThe ether is distilled off
  2. temperaturethe mixture refluxed for 48 hours
  3. temperatureheated on a steam bath for 1 hour
  4. extractionThe mixture is then extracted with ether
  5. dry with materialthe extract dried (MgSO4)
  6. concentrationconcentrated to an oil
  7. distillationDistillation of the oil in vacuo

출처 및 근거

ORD 기록
ord-342bd9d1a30e4660b58e6fb05d87e412
출처 데이터셋
uspto-grants-1979_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04143139

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