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

HRID 127086

反应方程式

HRID 127086 反应方程式
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]

参与物

6

反应物 4

HCID 795咪唑HCID 6228N,N-二甲基甲酰胺HCID 6397三甲基氯硅烷HCID 65251－乙炔基环己醇

产物 1

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

试剂、催化剂与溶剂 1

HCID 8058正己烷溶剂

实验过程

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.

后处理

  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-

来源与证据

ORD记录
ord-a1189e0ca4a44fd1bfba44c5ddbccffc
来源数据集
uspto-grants-1981_03
专利号
US04254285

关联笔记

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