1,3-Dibromopropane → 1-(3-Bromopropoxy)-4-fluorobenzene

HRID 467343

反応式

HRID 467343 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([OH:8])=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[Br:15][CH2:16][CH2:17][CH2:18]Br.C(COC)OC>C(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:18][CH2:17][CH2:16][Br:15])=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 80011,3-DibromopropaneHCID 80711,2-DimethoxyethaneHCID 97324-FluorophenolHCID 11430Potassium Carbonate

生成物 1

HCID 2600041-(3-Bromopropoxy)-4-fluorobenzene

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 11.2 g (0.1 mol) of 4-fluorophenol, 16.5 g (0.12 mol) of pulverized potassium carbonate, 20.2 g (0.1 mol) of 1,3-dibromopropane and 100 ml of anhydrous dimethoxyethane was refluxed under nitrogen for 6 hours and then cooled. The mixture was diluted with methylene chloride and washed with water. The resultant organic product solution was dried over Na2SO4 and evaporated in vacuo. The residue was chromatographed on silica gel using cyclohexane elution to give pure product.

後処理

  1. temperaturewas refluxed under nitrogen for 6 hours
  2. temperaturecooled
  3. washwashed with water
  4. dry with materialThe resultant organic product solution was dried over Na2SO4
  5. customevaporated in vacuo
  6. customThe residue was chromatographed on silica gel
  7. washcyclohexane elution
  8. customto give pure product

出典と根拠

ORDレコード
ord-60b5ca190a014fdba9710dfad12d80e0
出典データセット
uspto-grants-1992_10
特許番号
US05159097

関連ノート

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