咪唑 → tert-Butyl(2-fluorophenethoxy)dimethylsilane

HRID 471170

反应方程式

HRID 471170 反应方程式
[Si:1](Cl)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[F:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[CH2:16][CH2:17][OH:18].N1C=CN=C1>CN(C=O)C.C(OCC)(=O)C>[C:4]([Si:1]([O:18][CH2:17][CH2:16][C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[F:9])([CH3:3])[CH3:2])([CH3:7])([CH3:6])[CH3:5]

参与物

6

反应物 3

HCID 795咪唑HCID 28928叔丁基二甲基氯硅烷HCID 27332962-氟苯乙醇

产物 1

HCID 57988979tert-Butyl(2-fluorophenethoxy)dimethylsilane

试剂、催化剂与溶剂 2

HCID 6228N,N-二甲基甲酰胺溶剂HCID 8857乙酸乙酯溶剂

实验过程

tert-Butyldimethylsilyl chloride (6.45 g) was added to a stirred solution of 2-(2-fluorophenyl)ethanol (5.00 g) and 1H-imidazole (7.29 g) in dry DMF (30 mL) cooled in an ice bath. After 45 min, the reaction mixture was diluted with ethyl acetate, washed three times with water and evaporated in vacuo. The resulting gum was dissolved in isohexane and applied to a silica gel column eluting with isohexane followed by 1:3 ethyl acetate:isohexane to collect the product as an oil. Yield 9.0 g.

后处理

  1. temperaturecooled in an ice bath
  2. washwashed three times with water
  3. customevaporated in vacuo
  4. dissolutionThe resulting gum was dissolved in isohexane
  5. washeluting with isohexane
  6. customisohexane to collect the product as an oil

来源与证据

ORD记录
ord-75e7c65448fb44f4b8dc805bd90d4d62
来源数据集
uspto-grants-2014_01
专利号
US08629271B2

关联笔记

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