Potassium Hydroxide → 2'-Fluoro-2-((methyloxy)carbonyl)-1,1'-biphenyl-4-carboxylic acid

HRID 1662415노트

반응식

HRID 1662415 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[C:9]([C:18]([O:20][CH3:21])=[O:19])=[CH:10][C:11]([C:14]([O:16]C)=[O:15])=[CH:12][CH:13]=1.[OH-].[K+]>C1COCC1.CO>[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([C:14]([OH:16])=[O:15])=[CH:10][C:9]=1[C:18]([O:20][CH3:21])=[O:19]

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 57706591Dimethyl 2'-fluoro-1,1'-biphenyl-2,4-dicarboxylate

생성물 1

HCID 577067632'-Fluoro-2-((methyloxy)carbonyl)-1,1'-biphenyl-4-carboxylic acid수율 95%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 66.32A (1.00 g, 3.5 mmol) in THF (70.0 mL) and MeOH (70.0 mL) at 0° C. was slowly added potassium hydroxide (1.9 mL, 3.8 mmol) to maintain the temperature below 6° C. The reaction mixture was allowed to warm to room temperature and stirred for 48 hours. The reaction mixture was then concentrated in vacuo, acidified with 1N HCl, and extracted three times with EtOAc. After drying over anhydrous magnesium sulfate and filtering, the organic solvent was removed under reduced pressure and to give a white solid 66.32B (0.90 g, 95% yield).

후처리

  1. customat 0° C.
  2. temperatureto maintain the temperature below 6° C
  3. concentrationThe reaction mixture was then concentrated in vacuo
  4. extractionextracted three times with EtOAc
  5. dry with materialAfter drying over anhydrous magnesium sulfate
  6. filtrationfiltering
  7. customthe organic solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-96503ff0837841a9bc59ec8edb4b8a70
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030354B2

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