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

HRID 247661

反応式

HRID 247661 の反応式
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]

参加物

6

反応物 3

HCID 5943Carbon TetrachlorideHCID 184717Silane, (chloromethyl)(4-ethoxyphenyl)dimethyl-HCID 517045Sodium Acetate2 回

生成物 1

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

試薬・触媒・溶媒 2

HCID 70681Tetrabutylammonium Chloride触媒2 回HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c5694bf43ac44a9f9d99458ce32adaab
出典データセット
uspto-grants-1987_11
特許番号
US04709068

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