Hydrochloric Acid → HCID 178516151、化合物

HRID 1172092ノート

反応式

HRID 1172092 の反応式
[C:1]1([NH:7][NH2:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl.[F:10][C:11]([F:21])([F:20])[C:12](=O)[CH2:13][C:14](OCC)=[O:15]>C(O)C>[C:1]1([N:7]2[C:14]([OH:15])=[CH:13][C:12]([C:11]([F:21])([F:20])[F:10])=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 7516PhenylhydrazineHCID 67793Ethyl 4,4,4-trifluoroacetoacetate

生成物 1

HCID 178516151HCID 178516151、化合物収率 87.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

20 g (184.9 mmoles) of phenylhydrazine and 4 ml of concentrated hydrochloric acid were added to a solution of 34.1 g (184.9 mmoles) of ethyl trifluoroacetoacetate dissolved in 500 ml of ethanol. The mixture was refluxed for 1 hour with heating, to give rise to a reaction. After the completion of the reaction, the reaction mixture was subjected to vacuum distillation to remove the most part of the solvent contained therein. The residue was mixed with water to precipitate crystals. The crystals were collected by filtration, washed with water until the filtrate became neutral, and dried to obtain 37.1 g (yield: 87.9%) of 1-phenyl-3-trifluoromethyl-1H-pyrazol-5-ol as ocherous crystals.

後処理

  1. temperatureThe mixture was refluxed for 1 hour
  2. temperaturewith heating
  3. customto give rise
  4. customto a reaction
  5. customAfter the completion of the reaction
  6. distillationthe reaction mixture was subjected to vacuum distillation
  7. customto remove the most part of the solvent
  8. additionThe residue was mixed with water
  9. customto precipitate crystals
  10. filtrationThe crystals were collected by filtration
  11. washwashed with water until the filtrate
  12. customdried

出典と根拠

ORDレコード
ord-9a60088a76c1448b84b60816149a115f
出典データセット
uspto-grants-2010_11
特許番号
US07833939B2

反応ノート

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