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

HRID 247661

Reaktionsgleichung

Reaktionsgleichung von HRID 247661
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]

Komponenten

6

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-c5694bf43ac44a9f9d99458ce32adaab
Quelldatensatz
uspto-grants-1987_11
Patentnummer
US04709068

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