Citric Acid → 5-Methyl-1-[2'-(trifluoromethoxy)-1,1'-biphenyl-3-yl]-1H-pyrazole-3-carboxylic acid

HRID 733130노트

반응식

HRID 733130 반응식
C([O:3][C:4]([C:6]1[CH:10]=[C:9]([CH3:11])[N:8]([C:12]2[CH:13]=[C:14]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[O:24][C:25]([F:28])([F:27])[F:26])[CH:15]=[CH:16][CH:17]=2)[N:7]=1)=[O:5])C.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>CO.[OH-].[Na+].O>[CH3:11][C:9]1[N:8]([C:12]2[CH:13]=[C:14]([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[O:24][C:25]([F:28])([F:26])[F:27])[CH:15]=[CH:16][CH:17]=2)[N:7]=[C:6]([C:4]([OH:5])=[O:3])[CH:10]=1

참가 물질

6

반응물 2

HCID 311Citric AcidHCID 11417896Ethyl-5-methyl-1-[2'-(trifluoromethoxy)-1,1'-biphenyl-3-yl]-1H-pyrazole-3-carboxylate

생성물 1

HCID 112453825-Methyl-1-[2'-(trifluoromethoxy)-1,1'-biphenyl-3-yl]-1H-pyrazole-3-carboxylic acid

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 14798Sodium Hydroxide용매

실험 절차

A solution of ethyl-5-methyl-1-[2′-(trifluoromethoxy)-1,1′-biphenyl-3-yl]-1H-pyrazole-3-carboxylate (0.39 g, 1 mmol) (from EXAMPLE 3) in a mixture of MeOH (5 ml) and 2N NaOH (2 ml) was refluxed for 16 hours. The reaction was then cooled, diluted with water, acidified with 10% citric acid and extracted with ethylacetate. The organic phase was washed with water, dried (sodium sulfate) and concentrated in vacuo to give the titled product.

후처리

  1. temperaturewas refluxed for 16 hours
  2. temperatureThe reaction was then cooled
  3. extractionextracted with ethylacetate
  4. washThe organic phase was washed with water
  5. dry with materialdried (sodium sulfate)
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-c7e4ac8ac2f84f87b186de9e9e14f5b0
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07589116B2

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