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

HRID 225088

反应方程式

HRID 225088 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-ethynylcyclohexane-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-9ad67245796d45c799a8769bce276837
来源数据集
uspto-grants-1980_11
专利号
US04235797

关联笔记

加载中…