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Ethyl 4,4,4-trifluoroacetoacetate → HCID 178516161、化合物

HRID 1289852
ノート
印刷プレビュー

反応式

HRID 1289852 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 178516161HCID 178516161、化合物収率 33.8%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

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.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-db3e432a97484938bebc608c06dce22e
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05750550

反応ノート

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