1,1-Dichloroethane → 2-(4-Dodecanoylphenyl)ethyl acetate

HRID 617881노트

반응식

HRID 617881 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[C:5]([O:8][CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)(=[O:7])[CH3:6].[C:17](Cl)(=[O:28])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27].Cl[CH:31](Cl)C>>[C:5]([O:8][CH2:9][CH2:10][C:11]1[CH:16]=[CH:15][C:14]([C:17](=[O:28])[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:31])=[CH:13][CH:12]=1)(=[O:7])[CH3:6]

참가 물질

5

실험 절차

Aluminum chloride (48.2 g) was added to dichloroethane (400 ml) in a stream of nitrogen and the mixture was stirred at room temperature. Then, phenethyl acetate (39.6 g) and undecanoyl chloride (52.7 g) were dropwise added thereto under ice-cooling and the mixture was stirred at room temperature overnight. The reaction mixture was poured into ice water and extracted with diethyl ether. The ether layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was distilled away and the residue obtained was purified by silica gel column chromatography (eluent; ethyl acetate:hexane=1:20) to give the subject compound (34.5 g) as pale yellow crystals.

후처리

  1. temperatureunder ice-cooling
  2. stirringthe mixture was stirred at room temperature overnight
  3. extractionextracted with diethyl ether
  4. washThe ether layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled away
  7. customthe residue obtained
  8. customwas purified by silica gel column chromatography (eluent; ethyl acetate:hexane=1:20)

출처 및 근거

ORD 기록
ord-bcedc3e4f3f94ca7be74657317be12ec
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05952316

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