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

HRID 477790노트

반응식

HRID 477790 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-3efcb309c61045da9ed872907fc21c6c
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04889858

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