Acetic Acid → HCID 178516151, Verbindung

HRID 1159480

Reaktionsgleichung

Reaktionsgleichung von HRID 1159480
[F:1][C:2]([F:12])([F:11])[C:3](=O)[CH2:4][C:5]([O:7]CC)=O.C(O)(=O)C.[C:17]1([NH:23][NH2:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>O>[OH:7][C:5]1[N:23]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:24]=[C:3]([C:2]([F:1])([F:11])[F:12])[CH:4]=1

Komponenten

5

Edukt 3

HCID 176Acetic AcidHCID 7516PhenylhydrazineHCID 67793Ethyl 4,4,4-trifluoroacetoacetate

Produkt 1

HCID 178516151HCID 178516151, VerbindungAusbeute 98 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
10 °C

Versuchsvorschrift

18.4 g (0.1 mole) of ethyl 4,4,4-trifluoroacetoacetate was dissolved in 12.0 g (0.2 mole) of acetic acid. The solution was cooled to 10° C. or lower with stirring. Thereto was dropwise added, in 0.5 hour, 11.8 g (0.11 mole) of phenylhydrazine. After the dropwise addition, the mixture was stirred at room temperature for 1 hour and successively at 80° C. for 5 hours to give rise to a reaction. After the reaction, the mixture was cooled to room temperature. Thereto were added 100 ml of water. The resulting crystals were collected by filtration, washed with 50 ml of water twice, and dried in a hot-air drier, to obtain 22.3 g (yield: 98.0%) of a title compound as light yellow crystals.

Aufarbeitung

  1. additionThereto was dropwise added, in 0.5 hour
  2. additionAfter the dropwise addition
  3. stirringthe mixture was stirred at room temperature for 1 hour and successively at 80° C. for 5 hours
  4. customto give rise
  5. customto a reaction
  6. customAfter the reaction
  7. temperaturethe mixture was cooled to room temperature
  8. filtrationThe resulting crystals were collected by filtration
  9. washwashed with 50 ml of water twice
  10. customdried in a hot-air drier,

Quellen und Nachweise

ORD-Eintrag
ord-ccef4bbee4aa4a869de99b8b2947ce1a
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07812175B2

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