Carbon Tetrachloride → 2-(4-Ethoxyphenyl)-2-methyl-2-silapropyl acetate

HRID 247661

반응식

HRID 247661 반응식
Cl[CH2:2][Si:3]([C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH3:14])=[CH:8][CH:7]=1)([CH3:5])[CH3:4].[C:15]([O-:18])(=[O:17])[CH3:16].[Na+].C(Cl)(Cl)(Cl)Cl>[Cl-].C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)C>[C:15]([O:18][CH2:2][Si:3]([C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH3:14])=[CH:8][CH:7]=1)([CH3:5])[CH3:4])(=[O:17])[CH3:16]

참가 물질

6

반응물 3

HCID 5943Carbon TetrachlorideHCID 184717Silane, (chloromethyl)(4-ethoxyphenyl)dimethyl-HCID 517045Sodium Acetate2회

생성물 1

HCID 140144832-(4-Ethoxyphenyl)-2-methyl-2-silapropyl acetate수율 105.4%

시약·촉매·용매 2

HCID 70681Tetrabutylammonium Chloride촉매2회HCID 3283Diethyl Ether용매

실험 절차

In a flask under nitrogen were placed 10.1 g (0.044 mole) of (chloromethyl)(4-ethoxyphenyl)dimethylsilane, 4.0 g (0.049 mole) of sodium acetate, 1.2 g (0.0043 mole) of tetrabutylammonium chloride, and 75 ml of carbon tetrachloride. This mixture was refluxed for four days. After cooling to room temperature, 2.0 g (0.024 mole) of sodium acetate and 0.60 g (0.0022 mole) of tetrabutylammonium chloride was added, and the reaction mixture was refluxed for five more days. This mixture was then diluted with diethyl ether, filtered through silica gel, and the solvent was evaporated under reduced pressure, leaving 11.7 g of 2-(4-ethoxyphenyl)-2-methyl-2-silapropyl acetate as a clear, light brown oil. The nmr spectrum was consistent with the proposed structure.

후처리

  1. customIn a flask under nitrogen were placed
  2. temperatureThis mixture was refluxed for four days
  3. temperaturethe reaction mixture was refluxed for five more days
  4. filtrationfiltered through silica gel
  5. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-c5694bf43ac44a9f9d99458ce32adaab
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04709068

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