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

HRID 733130ノート

反応式

HRID 733130 の反応式
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

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c7e4ac8ac2f84f87b186de9e9e14f5b0
出典データセット
uspto-grants-2009_09
特許番号
US07589116B2

反応ノート

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