Methanol → Cyclohexyl(dimethoxy)(2-methylpropyl)silane

HRID 1032495

반응식

HRID 1032495 반응식
[CH2:1]([Si:5](OC)([O:8][CH3:9])[O:6][CH3:7])[CH:2]([CH3:4])[CH3:3].[CH:12]1([Mg]Cl)[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1.CO>C(OCC)C>[CH2:1]([Si:5]([CH:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1)([O:8][CH3:9])[O:6][CH3:7])[CH:2]([CH3:4])[CH3:3]

참가 물질

5

반응물 3

HCID 887MethanolHCID 87622IsobutyltrimethoxysilaneHCID 178478990HCID 178478990, 화합물

생성물 1

HCID 14513104Cyclohexyl(dimethoxy)(2-methylpropyl)silane

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

Under an inert gas, 152.0 g isobutyltrimethoxy silane (0.85 mol) was dissolved in 50 ml diethylether. While stirring, 667 ml of a 1.5 molar solution of cyclohexylmagnesiumchloride in ether was added dropwise to the solution at a rate to maintain a moderate reflux. At the end of the addition, the reaction was continued under reflux for several hours. After cooling the reaction mixture, 4.8 g methanol (0.15 mol) was added, stirred for a few minutes and then the resulting precipitate was removed by filtration. The filter cake was washed with several portions of diethylether. The solvent was then evaporated from the combined filtrates using a water aspirator. The remaining residue consisted of 192.7 g (98.4% of the theoretical yield) isobutylcyclohexyldimethoxysilane, which had a purity of 98% according to gas chromatography (GC). Isobutyldicyclohexylmethoxysilane was not detected by GC.

후처리

  1. temperatureto maintain a moderate reflux
  2. additionAt the end of the addition
  3. temperatureunder reflux for several hours
  4. additionwas added
  5. stirringstirred for a few minutes
  6. customthe resulting precipitate was removed by filtration
  7. washThe filter cake was washed with several portions of diethylether
  8. customThe solvent was then evaporated from the combined filtrates

출처 및 근거

ORD 기록
ord-f160e0cae8d04cdc8640ecb701541517
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04958041

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