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Ethyl 4,4,4-trifluoroacetoacetate → HCID 178516161, 화합물

HRID 1289852
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HRID 1289852 반응식
[NH:1]([C:3]1[N:8]=[CH:7][CH:6]=[CH:5][N:4]=1)[NH2:2].[F:9][C:10]([F:20])([F:19])[C:11](=O)[CH2:12][C:13](OCC)=[O:14]>C(O)(=O)C>[N:4]1[CH:5]=[CH:6][CH:7]=[N:8][C:3]=1[N:1]1[C:13]([OH:14])=[CH:12][C:11]([C:10]([F:20])([F:19])[F:9])=[N:2]1
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참가 물질

4

반응물 2

HCID 67793Ethyl 4,4,4-trifluoroacetoacetateHCID 3465582-Hydrazinylpyrimidine

생성물 1

HCID 178516161HCID 178516161, 화합물수율 33.8%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of 2 g (9 mmol) of 2-hydrazinopyrimidine and ethyl trifluoroacetoacetate (2.6 ml; 9.1 mmol) in 10 ml of acetic acid was refluxed for 60 hours with stirring under nitrogen and then cooled. The mixture was concentrated in vacuo, the residue was diluted with 100 ml of water, and the mixture was extracted with ethyl acetate (3×). The combined organic layer was dried over magnesium sulfate, and concentrated in vacuo. The resulting residue was dried in vacuo to afford 700 mg of 1-(2-pyrimidinyl)-3-trifluoromethyl-5-hydroxypyrazole as a red gum.

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후처리

  1. temperaturewas refluxed for 60 hours
  2. temperaturecooled
  3. concentrationThe mixture was concentrated in vacuo
  4. additionthe residue was diluted with 100 ml of water
  5. extractionthe mixture was extracted with ethyl acetate (3×)
  6. dry with materialThe combined organic layer was dried over magnesium sulfate
  7. concentrationconcentrated in vacuo
  8. customThe resulting residue was dried in vacuo

출처 및 근거

ORD 기록
ord-db3e432a97484938bebc608c06dce22e
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05750550

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