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

HRID 494195

반응식

HRID 494195 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2d6bde3cad07401a9de0ebff325799d2
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07538121B2

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