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

HRID 1032496

反応式

HRID 1032496 の反応式
[Mg].II.[CH:4]1(Cl)[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1.[CH2:11]([Si:15](OC)([O:18][CH3:19])[O:16][CH3:17])[CH:12]([CH3:14])[CH3:13].CO>COC(C)(C)C>[CH2:11]([Si:15]([CH:4]1[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1)([O:18][CH3:19])[O:16][CH3:17])[CH:12]([CH3:14])[CH3:13]

参加物

7

反応物 5

HCID 807IodineHCID 887MethanolHCID 10952Chlorocyclohexane2 回HCID 87622IsobutyltrimethoxysilaneHCID 5462224Magnesium

生成物 1

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

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒2 回

実験手順

Under an inert gas, 24.3 g magnesium chips (1.0 mol) were combined with about 10 ml methyl-tert-butylether, an iodine crystal and 3.6 g cyclohexylchloride (0.03 mol). To start the reaction, a solution of 152.0 g isobutyltrimethoxysilane (0.85 mol) and 115.0 g cyclohexylchloride (0.97 mol) in 130 ml methyl-tert-butylether was added dropwise, with stirring, to the first mixture at a rate to maintain a moderate reflux. At the end of this addition, the reaction was allowed to reflux for two more hours. After cooling the reaction mixture, 4.8 g methanol (0.15 mol) was added, stirred for a few minutes and then the precipitate was removed by filtration. The filter cake was washed with several portions of methyl-tert-butylether. The solvent was evaporated from the combined filtrates by water vacuum. The remaining residue consisted of 192.5 g (98.4% of the theoretical yield) isobutylcyclohexyldimethoxysilane which had a purity of 98% according to GC. Isobutyldicyclohexylmethoxysilane was not detected by GC.

後処理

  1. customthe reaction
  2. temperatureto maintain a moderate reflux
  3. additionAt the end of this addition
  4. temperatureto reflux for two more hours
  5. additionwas added
  6. stirringstirred for a few minutes
  7. customthe precipitate was removed by filtration
  8. washThe filter cake was washed with several portions of methyl-tert-butylether
  9. customThe solvent was evaporated from the combined filtrates by water vacuum

出典と根拠

ORDレコード
ord-a26ad30f1f404dbca25184fe25d06c96
出典データセット
uspto-grants-1990_09
特許番号
US04958041

関連ノート

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