Hydrochloric Acid → 2',5'-Difluoro-2-((methyloxy)carbonyl)-1,1'-biphenyl-4-carboxylic acid

HRID 1662546노트

반응식

HRID 1662546 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[C:9]1[C:10]([C:19]([O:21][CH3:22])=[O:20])=[CH:11][C:12]([C:15]([O:17]C)=[O:16])=[CH:13][CH:14]=1.[OH-].[K+].Cl>C1COCC1.CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([F:8])=[CH:4][C:3]=1[C:9]1[CH:14]=[CH:13][C:12]([C:15]([OH:17])=[O:16])=[CH:11][C:10]=1[C:19]([O:21][CH3:22])=[O:20]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 57707138Dimethyl 2',5'-difluoro-1,1'-biphenyl-2,4-dicarboxylate

생성물 1

HCID 577063522',5'-Difluoro-2-((methyloxy)carbonyl)-1,1'-biphenyl-4-carboxylic acid수율 100%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

To a stirred solution of 83.27A (0.800 g, 2.6 mmol) in THF (7.00 mL) and MeOH (7.00 mL) at 0° C. was slowly added potassium hydroxide (1.4 mL, 2.9 mmol) to maintain the temperature below 6° C. The reaction mixture was then allowed to warm to room temperature and stirred for 19 hours. The reaction was then 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 to yield 83.27B as a colorless solid (0.76 g, 100% yield).

후처리

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

출처 및 근거

ORD 기록
ord-e9a4f0a4b1344172958b7c7db58c5b00
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030354B2

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