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Hydrochloric Acid → HCID 178463142、化合物

HRID 854130
ノート
印刷プレビュー

反応式

HRID 854130 の反応式
[CH2:1]([NH:3][NH2:4])[CH3:2].[F:5][C:6]([F:17])([F:16])[C:7](=O)[CH:8]([CH3:14])[C:9](OCC)=[O:10].Cl>C(O)C>[CH2:1]([N:3]1[C:9]([OH:10])=[C:8]([CH3:14])[C:7]([C:6]([F:17])([F:16])[F:5])=[N:4]1)[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 29062EthylhydrazineHCID 2737204Ethyl 2-methyl-4,4,4-trifluoroacetoacetate

生成物 1

HCID 178463142HCID 178463142、化合物収率 72.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 1.2 g (20.0 mmol) of ethylhydrazine in 20 ml of ethanol was added dropwise under stirring 4.4 g (20.0 mmol) of ethyl 4,4,4-trifluoro-2-methyl-3-oxobutanoate under ice-cooling so that the temperature in the reaction system did not exceed 10° C. After the dropwise addition, the whole was stirred at room temperature for 30 minutes. Then, 1 ml of concentrated hydrochloric acid was added into the reaction solution, followed by 2 days of stirring under refluxing. After the completion of the reaction was confirmed, the solvent was removed by evaporation under reduced pressure. Water was added to the residue, followed by extraction with ethyl acetate. The resulting organic layer was washed with water and saline, successively, and then dried over anhydrous magnesium sulfate. The solvent was removed by evaporation under reduced pressure and the residue was washed with n-hexane to obtain 2.8 g (yield: 71.8%) of 1-ethyl-5-hydroxy-4-methyl-3-trifluoromethyl-1H-pyrazole as white crystals (melting point: 150 to 152° C.).

後処理

  1. temperaturecooling so that the temperature in the reaction system
  2. customdid not exceed 10° C
  3. additionAfter the dropwise addition
  4. waitfollowed by 2 days
  5. stirringof stirring
  6. temperatureunder refluxing
  7. customthe solvent was removed by evaporation under reduced pressure
  8. additionWater was added to the residue
  9. extractionfollowed by extraction with ethyl acetate
  10. washThe resulting organic layer was washed with water and saline
  11. dry with materialsuccessively, and then dried over anhydrous magnesium sulfate
  12. customThe solvent was removed by evaporation under reduced pressure
  13. washthe residue was washed with n-hexane

出典と根拠

ORDレコード
ord-66e9e2f25c484925a6feb167904cece1
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07256298B2

反応ノート

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