Water → HCID 14626274、化合物

HRID 477787ノート

反応式

HRID 477787 の反応式
[Na].[F:2][C:3]1[CH:4]=[C:5]([OH:9])[CH:6]=[CH:7][CH:8]=1.[F:10][C:11]1[C:12]([CH2:22]Br)=[C:13]([CH:19]=[CH:20][CH:21]=1)[C:14]([O:16][CH2:17][CH3:18])=[O:15].O>C(O)C>[F:10][C:11]1[C:12]([CH2:22][O:9][C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([F:2])[CH:4]=2)=[C:13]([CH:19]=[CH:20][CH:21]=1)[C:14]([O:16][CH2:17][CH3:18])=[O:15]

参加物

6

反応物 4

HCID 962WaterHCID 97433-FluorophenolHCID 5360545SodiumHCID 14626273Ethyl 2-(bromomethyl)-3-fluorobenzoate

生成物 1

HCID 14626274HCID 14626274、化合物収率 89.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 1.3 g of sodium metal in 100 ml of ethanol are added 6.3 g of 3-fluorophenol and 13 g of ethyl 3-fluoro-2-bromomethylbenzoate and the mixture is refluxed with heating for 8 hours. After cooling, 300 ml of water is added and the mixture is extracted with toluene. After the extract is washed with water and a saturated saline solution and dried over magnesium sulfate, the solvent is distilled off under reduced pressure. The residue is subjected to silica-gel chromatography and eluted with toluene to give 13 g of ethyl 3-fluoro-2-[(3-fluorophenyl oxy)methyl]benzoate (oil). Mass spectrum m/z: 292(M+).

後処理

  1. temperaturethe mixture is refluxed
  2. temperaturewith heating for 8 hours
  3. temperatureAfter cooling
  4. extractionthe mixture is extracted with toluene
  5. washAfter the extract is washed with water
  6. dry with materiala saturated saline solution and dried over magnesium sulfate
  7. distillationthe solvent is distilled off under reduced pressure
  8. washeluted with toluene

出典と根拠

ORDレコード
ord-f90bf39688424761bedb7c925ef97d34
出典データセット
uspto-grants-1989_12
特許番号
US04889858

反応ノート

読み込み中…