Sodium Hydroxide → HCID 23499547、化合物

HRID 1251882ノート

反応式

HRID 1251882 の反応式
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([O:9]C)=[O:8])=[C:5]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[CH:4]=1.[OH-].[Na+]>CO>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:6]([C:7]([OH:9])=[O:8])=[C:5]([C:13]2[CH:18]=[CH:17][C:16]([F:19])=[CH:15][CH:14]=2)[CH:4]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 23499548Methyl 4-methoxy-2-(4-fluorophenyl)benzoate

生成物 1

HCID 23499547HCID 23499547、化合物収率 107.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of methyl 4-methoxy-2-(4-fluorophenyl)benzoate (9.8 g; 0.029 mol) in methanol (75 ml) was added 2N aqueous sodium hydroxide solution (45 ml) and the mixture heated at reflux for 1.5 h. The reaction was cooled to ambient temperature, filtered and the filtrate concentrated in vacuo to remove the methanol. The residual aqueous phase was washed with diethyl ether, acidified to pH 1 with concentrated HCl and extracted with ethyl acetate. The organic extracts were dried (MgSO4) and the solvent removed in vacuo to give 4-methoxy-2-(4-fluorophenyl)benzoic acid as a white solid (7.7 g), which was used without further purification.

後処理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 1.5 h
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated in vacuo
  5. customto remove the methanol
  6. washThe residual aqueous phase was washed with diethyl ether
  7. extractionextracted with ethyl acetate
  8. dry with materialThe organic extracts were dried (MgSO4)
  9. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-04662595b38149218818428512bf04e4
出典データセット
uspto-grants-2002_01
特許番号
US06342765B1

反応ノート

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