4-Chlorophenylhydrazine sulfate → 2-[1-(4-chlorophenyl)-3,5-dimethyl-1H-pyrazol-4-yl]acetic acid

HRID 615006노트

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HRID 615006 반응식
[C:1]([CH:4]([C:9](=O)[CH3:10])[CH2:5][C:6]([OH:8])=[O:7])(=O)[CH3:2].[CH:12]1[C:17]([NH:18][NH2:19])=[CH:16][CH:15]=[C:14]([Cl:20])[CH:13]=1.OS(O)(=O)=O.C([O-])(=O)C.[Na+]>C(O)(=O)C>[CH3:2][C:1]1[C:4]([CH2:5][C:6]([OH:8])=[O:7])=[C:9]([CH3:10])[N:18]([C:17]2[CH:16]=[CH:15][C:14]([Cl:20])=[CH:13][CH:12]=2)[N:19]=1

참가 물질

5

반응물 3

HCID 1124254-Chlorophenylhydrazine sulfateHCID 517045Sodium AcetateHCID 217146503-Acetyl-4-oxopentanoic acid

생성물 1

HCID 167736872-[1-(4-chlorophenyl)-3,5-dimethyl-1H-pyrazol-4-yl]acetic acid수율 102%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
60 °C

실험 절차

4.0 grams 3,3-diacetyl-propionic acid, 4.9 grams p-chlorophenylhydrazine-sulfate, 2.1 grams anhydrous sodium acetate and 30 milliliters glacial acetic acid were mixed and the mixture was heated to 60° C. for 3 hours. The reaction mixture was evaporated and water was added to the residue. The precipitate formed thereby was separated by filtration and recrystallized from a mixture of ethanol and of water. 5.5 grams 3,5-dimethyl-1-(p-chlorophenyl)-pyrazol-4-acetic acid, melting at 176°-177° C., were obtained, representing a yield of 82%.

후처리

  1. customThe reaction mixture was evaporated
  2. additionwater was added to the residue
  3. customThe precipitate formed
  4. customthereby was separated by filtration
  5. customrecrystallized from a mixture of ethanol and of water

출처 및 근거

ORD 기록
ord-85c8bcc668174d689adaae1b3411f4d9
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04146721

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