咪唑 → tert-Butyl(2-fluorophenethoxy)dimethylsilane

HRID 446361

反应方程式

HRID 446361 反应方程式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][CH2:9][OH:10].N1C=CN=C1.[C:16]([Si:20]([CH3:23])([CH3:22])Cl)([CH3:19])([CH3:18])[CH3:17]>CN(C=O)C>[C:16]([Si:20]([O:10][CH2:9][CH2:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[F:1])([CH3:23])[CH3:22])([CH3:19])([CH3:18])[CH3:17]

参与物

5

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 1

HCID 6228N,N-二甲基甲酰胺溶剂

实验过程

A solution of 2-(2-fluorophenyl)ethanol (5.5 g) and imidazole (8.0 g) in DMF (50 mL) was cooled in ice-water, treated with tert-butyldimethylchlorosilane (6.52 g), then removed as from the cooling bath and stirred at room temperature for 3.5 hours. The solution was poured into water and extracted three times with diethyl ether. The combined organic extracts were washed three times with water, once with brine, then dried over anhydrous magnesium sulphate and concentrated under reduced pressure to afford the subtitled compound as a colourless oil. Yield 9.9 g.

后处理

  1. customremoved as from the cooling bath
  2. additionThe solution was poured into water
  3. extractionextracted three times with diethyl ether
  4. washThe combined organic extracts were washed three times with water
  5. dry with materialonce with brine, then dried over anhydrous magnesium sulphate
  6. concentrationconcentrated under reduced pressure

来源与证据

ORD记录
ord-8f60e07498774f7a95a9ed9eff840734
来源数据集
uspto-grants-2013_07
专利号
US08476265B2

关联笔记

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