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Hydrochloric Acid → HCID 178492075, 화합물

HRID 1289840
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HRID 1289840 반응식
[F:1][C:2]([F:12])([F:11])[C:3](=O)[CH2:4][C:5]([O:7]CC)=O.Cl.[CH3:14][O:15][C:16]1[CH:21]=[CH:20][C:19]([NH:22][NH2:23])=[CH:18][CH:17]=1.Cl>CO>[CH3:14][O:15][C:16]1[CH:21]=[CH:20][C:19]([N:22]2[C:5]([OH:7])=[CH:4][C:3]([C:2]([F:1])([F:11])[F:12])=[N:23]2)=[CH:18][CH:17]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 67793Ethyl 4,4,4-trifluoroacetoacetateHCID 27239044-Methoxyphenylhydrazine hydrochloride

생성물 1

HCID 178492075HCID 178492075, 화합물수율 53%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 5 g (27.2 mmol) of ethyl trifluoroacetoacetate, 4.76 g (27.2 mmol) of 4-methoxyphenylhydrazine hydrochloride, and 0.5 ml of conc. HCl in 60 ml of methanol was refluxed with stirring for 22 hours. After removing methanol in vacuo, toluene was added and the resulting mixture was refluxed for 20 hours and cooled. The mixture was diluted with aqueous sodium bicarbonate solution, extracted with ethyl acetate, and the organic layer was dried over sodium sulfate and concentrated in vacuo. The residue was recrystallized from methylene chloride/hexane and ethyl acetate/hexane to afford 3.7 g (53%) of 1-(4-methoxyphenyl)-3-trifluoromethyl-5-hydroxypyrazole as a tan solid.

후처리

  1. temperaturewas refluxed
  2. customAfter removing methanol in vacuo, toluene
  3. additionwas added
  4. temperaturethe resulting mixture was refluxed for 20 hours
  5. temperaturecooled
  6. additionThe mixture was diluted with aqueous sodium bicarbonate solution
  7. extractionextracted with ethyl acetate
  8. dry with materialthe organic layer was dried over sodium sulfate
  9. concentrationconcentrated in vacuo
  10. customThe residue was recrystallized from methylene chloride/hexane and ethyl acetate/hexane

출처 및 근거

ORD 기록
ord-9fec037b9b3f448faa894baad5833020
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05750550

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