Ammonia → HCID 53905449, Verbindung

HRID 2285981Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2285981
[C:1]1([N:7]2[C:11]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)=[C:10]([CH2:18][C:19]([OH:21])=O)[C:9]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)(Cl)=O.[NH3:33].O>C1C=CC=CC=1.C(OC(=O)C)C>[C:1]1([N:7]2[C:11]([C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=3)=[C:10]([CH2:18][C:19]([NH2:33])=[O:21])[C:9]([C:22]3[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=3)=[N:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Komponenten

7

Edukt 4

HCID 222AmmoniaHCID 962WaterHCID 24813Phosphorus oxychlorideHCID 3084566Trifezolac

Produkt 1

HCID 53905449HCID 53905449, VerbindungAusbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 241BenzeneLösungsmittel2×HCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

3.54 grams 1,3,5-triphenyl-pyrazol-4-acetic acid, 1.68 gram phosphorus oxychloride and 30 milliliters benzene were mixed and the mixture heated to the boiling temperature under reflux for 2 hours. The reaction mixture, containing in benzene solution the correspondingly substituted acetyl chloride was then added dropwise at 0° C. to 30 milliliters 25% aqueous ammonia solution. The mixture was permitted to stand over night at room temperature. Thereafter, 30 milliliteres water and enough ethylacetate were added to cause dissolution of the crystalline mass formed in the reaction mixture. The organic phase was separated, dried with magnesium sulfate, evaporated and the residue was recrystallized from a mixture of ethanol and water. 3.2 grams 1,3,5-triphenyl-pyrazol-4-acetamide, melting at 207°-207.5° C., were obtained, representing a yield of 91%.

Aufarbeitung

  1. temperaturethe mixture heated to the boiling temperature
  2. temperatureunder reflux for 2 hours
  3. waitto stand over night at room temperature
  4. dissolutiondissolution of the crystalline mass
  5. customformed in the reaction mixture
  6. customThe organic phase was separated
  7. dry with materialdried with magnesium sulfate
  8. customevaporated
  9. customthe residue was recrystallized from a mixture of ethanol and water

Quellen und Nachweise

ORD-Eintrag
ord-c30e8f01477b4744ac8009b93430db1f
Quelldatensatz
uspto-grants-1982_04
Patentnummer
US04325962

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