Hydrochloric Acid → HCID 178516151, Verbindung

HRID 1172092

Reaktionsgleichung

Reaktionsgleichung von HRID 1172092
[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

Komponenten

5

Edukt 3

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

Produkt 1

HCID 178516151HCID 178516151, VerbindungAusbeute 87,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-9a60088a76c1448b84b60816149a115f
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07833939B2

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