Imidazole → tert-Butyl(2-fluorophenethoxy)dimethylsilane

HRID 471170

反応式

HRID 471170 の反応式
[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]

参加物

6

反応物 3

HCID 795ImidazoleHCID 28928tert-Butyldimethylsilyl chlorideHCID 27332962-(2-Fluorophenyl)ethan-1-ol

生成物 1

HCID 57988979tert-Butyl(2-fluorophenethoxy)dimethylsilane

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-75e7c65448fb44f4b8dc805bd90d4d62
出典データセット
uspto-grants-2014_01
特許番号
US08629271B2

関連ノート

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