Sodium Hydroxide → 4'-Fluoro-2-(2-methoxyethoxy)-1,1'-biphenyl-4-carboxylic acid

HRID 494195ノート

反応式

HRID 494195 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:13]=[CH:12][C:11]([C:14]([O:16]C)=[O:15])=[CH:10][C:9]=2[O:18][CH2:19][CH2:20][O:21][CH3:22])=[CH:4][CH:3]=1.[OH-].[Na+]>C(O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:13]=[CH:12][C:11]([C:14]([OH:16])=[O:15])=[CH:10][C:9]=2[O:18][CH2:19][CH2:20][O:21][CH3:22])=[CH:6][CH:7]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 69039439Methyl 4'-fluoro-2-(2-methoxyethoxy)-1,1'-biphenyl-4-carboxylate

生成物 1

HCID 690396114'-Fluoro-2-(2-methoxyethoxy)-1,1'-biphenyl-4-carboxylic acid収率 11.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Methyl 4′-fluoro-2-(2-methoxyethoxy)-1,1′-biphenyl-4-carboxylate (D76) (494 mg) was treated with aq. 2M sodium hydroxide solution (2 ml) in ethanol (3 ml) at 90° C. overnight. After cooling, the ethanol was evaporated off and the residue dissolved in EtOAc and extracted with sat. aq. sodium bicarbonate solution. This was acidified to pH3 with 2M HCl and extracted with EtOAc which was dried over MgSO4 and concentrated in vacuo to give the title compound as a solid (55 mg). MS(ES): M-H+ 289.

後処理

  1. temperatureAfter cooling
  2. customthe ethanol was evaporated off
  3. dissolutionthe residue dissolved in EtOAc
  4. extractionextracted with sat. aq. sodium bicarbonate solution
  5. extractionextracted with EtOAc which
  6. dry with materialwas dried over MgSO4
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2d6bde3cad07401a9de0ebff325799d2
出典データセット
uspto-grants-2009_05
特許番号
US07538121B2

反応ノート

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