Ethanol → HCID 21503217、化合物

HRID 1287963

反応式

HRID 1287963 の反応式
[Na].[C:2]1([P:8](Cl)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:16]([Si:18]([O:25][CH2:26][CH3:27])([O:22][CH2:23][CH3:24])[O:19][CH2:20][CH3:21])=[CH2:17].C([SiH3])=C.C([OH:33])C>C1(C)C=CC=CC=1>[C:2]1([P:8]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)([CH2:17][CH2:16][Si:18]([O:19][CH2:20][CH3:21])([O:25][CH2:26][CH3:27])[O:22][CH2:23][CH3:24])=[O:33])[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:9]1([PH:8][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

参加物

8

反応物 5

HCID 702EthanolHCID 6516VinyltriethoxysilaneHCID 66180ChlorodiphenylphosphineHCID 81714VinylsilaneHCID 5360545Sodium

生成物 2

HCID 70017Diphenylphosphine収率 16.3%HCID 21503217HCID 21503217、化合物収率 16.7%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a suspension of sodium diphenylphosphide prepared, under nitrogen in dry toluene (100 ml), from sodium (4.6, 0.2 g atom) and diphenylphosphinous chloride (22.0 g, 0.1 mol), vinyl triethoxysilane (19.0 g, 0.1 mol) is added during 45 minutes. A slight temperature rise occurs. The temperature is held at 30° C by adjusting the feed rate of the vinyl silane. After 3 hours, 5 ml anhydrous ethanol is added. The yellow color of the anion is instantly discharged. The solution is filtered to remove inorganic salts. Gas chromatographic analysis confirms the presence of diphenyl phosphine and 2-(dipenylphosphinyl)ethyl triethoxysilane. After neutralization with carbon dioxide, the liquid is distilled giving 6.3 g (16.7 percent yield) of 2-(diphenylphosphinyl) ethyl triethoxysilane and 3.0 g (16.3 percent yield) of diphenylphosphine. The H'NMR spectrum of the silane is identical to that of the product of addition of diphenylphosphine to vinyl triethoxysilane with a radical initiator.

後処理

  1. additionis added during 45 minutes
  2. customis held at 30° C
  3. filtrationThe solution is filtered
  4. customto remove inorganic salts
  5. distillationAfter neutralization with carbon dioxide, the liquid is distilled

出典と根拠

ORDレコード
ord-3a1a5d85b97544fc8c317f13b16ea707
出典データセット
uspto-grants-1976_10
特許番号
US03987009

関連ノート

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