Imidazole → Silane, [(1-ethynylcyclohexyl)oxy]trimethyl-

HRID 127086

反応式

HRID 127086 の反応式
N1C=CN=C1.[C:6]([C:8]1([OH:14])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1)#[CH:7].CN(C)C=O.[CH3:20][Si:21]([CH3:24])([CH3:23])Cl>CCCCCC>[C:6]([C:8]1([O:14][Si:21]([CH3:24])([CH3:23])[CH3:20])[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1)#[CH:7]

参加物

6

反応物 4

HCID 795ImidazoleHCID 6228DimethylformamideHCID 6397ChlorotrimethylsilaneHCID 65251-Ethynylcyclohexanol

生成物 1

HCID 552482Silane, [(1-ethynylcyclohexyl)oxy]trimethyl-

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

A 194 g portion of imidazole and 158.2 g of 1-ethynylcyclohexan-1-ol are mixed with 500 g of dimethylformamide with cooling in an ice bath. A 152 g portion of trimethylchlorosilane is added with cooling and stirring in about one minute. The mixture is stirred for one hour and allowed to stand overnight. One liter of hexane is added. The lower layer is separated, diluted with water and extracted with hexane. The hexane layers are washed several times with water and then combined and dried over magnesium sulfate. Filtration and then evaporation of the hexane-gives 198.5 g of product which is distilled giving 168 g of the desired product.

後処理

  1. temperaturewith cooling in an ice bath
  2. temperaturewith cooling
  3. stirringThe mixture is stirred for one hour
  4. waitto stand overnight
  5. customThe lower layer is separated
  6. additiondiluted with water
  7. extractionextracted with hexane
  8. washThe hexane layers are washed several times with water
  9. dry with materialdried over magnesium sulfate
  10. filtrationFiltration
  11. customevaporation of the hexane-

出典と根拠

ORDレコード
ord-a1189e0ca4a44fd1bfba44c5ddbccffc
出典データセット
uspto-grants-1981_03
特許番号
US04254285

関連ノート

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