Methanol → HCID 20542689, Verbindung

HRID 2285979Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2285979
[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:20])[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.[CH3:28]O.S(=O)(=O)(O)O>C(Cl)(Cl)(Cl)Cl>[CH3:28][O:20][C:19](=[O:21])[CH2:18][C:10]1[C:9]([C:22]2[CH:23]=[CH:24][CH:25]=[CH:26][CH:27]=2)=[N:8][N:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:11]=1[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

Komponenten

5

Edukt 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 3084566Trifezolac

Produkt 1

HCID 20542689HCID 20542689, VerbindungAusbeute 91 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 5943Carbon TetrachlorideLösungsmittel

Versuchsvorschrift

15 grams 1,3,5-triphenyl-pyrazol-4-acetic acid, 50 milliliters methanol, 40 milliliters carbon tetrachloride and 0.64 gram concentrated sulfuric acid were mixed and the mixture heated to the boiling temperature under reflux for 11 hours. The cooled reaction mixture was then extracted, first with sodium carbonate solution and thereafter with water. The organic phase was then dried and evaporated. The residue was recrystallized from a mixture of methanol and water. 14.2 grams 1,3,5-triphenylpyrazol-4-acetic acid-methyl ester, melting at 80.5°-81.5° C., were obtained, representing a yield of 91%.

Aufarbeitung

  1. temperaturethe mixture heated to the boiling temperature
  2. temperatureunder reflux for 11 hours
  3. customThe cooled reaction mixture
  4. extractionwas then extracted, first with sodium carbonate solution
  5. customThe organic phase was then dried
  6. customevaporated
  7. customThe residue was recrystallized from a mixture of methanol and water

Quellen und Nachweise

ORD-Eintrag
ord-3066bb22df1f4180bb96bb7a92190eb9
Quelldatensatz
uspto-grants-1982_04
Patentnummer
US04325962

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