Water → Ethyl 5-fluoro-2-[(3-fluorophenyloxy)methyl]benzoate

HRID 477790ノート

反応式

HRID 477790 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[CH:12]=[CH:13][C:14]([CH2:22]Br)=[C:15]([CH:21]=1)[C:16]([O:18][CH2:19][CH3:20])=[O:17].O>C(O)C>[F:10][C:11]1[CH:12]=[CH:13][C:14]([CH2:22][O:9][C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([F:2])[CH:4]=2)=[C:15]([CH:21]=1)[C:16]([O:18][CH2:19][CH3:20])=[O:17]

参加物

6

反応物 4

HCID 962WaterHCID 97433-FluorophenolHCID 5360545SodiumHCID 14626277Ethyl 2-(bromomethyl)-5-fluorobenzoate

生成物 1

HCID 14626278Ethyl 5-fluoro-2-[(3-fluorophenyloxy)methyl]benzoate収率 105.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 1.5 g of sodium metal in 100 ml of ethanol are added 8 g of 3-fluorophenol and 17 g of ethyl 5-fluoro-2-bromomethylbenzoate [U.S. Pat. No. 4,082,850]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. The extract is washed with water and a saturated saline solution and dried over magnesium sulfate. The solvent is distilled off under reduced pressure to give 20 g of ethyl 5-fluoro-2-[(3-fluorophenyl oxy)methyl]benzoate (oil). Mass spectrum m/z: 292(M+).

後処理

  1. temperature4,082,850]and the mixture is refluxed
  2. temperaturewith heating for 8 hours
  3. temperatureAfter cooling
  4. extractionthe mixture is extracted with toluene
  5. washThe 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

出典と根拠

ORDレコード
ord-3efcb309c61045da9ed872907fc21c6c
出典データセット
uspto-grants-1989_12
特許番号
US04889858

反応ノート

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