Ammonia → HCID 178481735, Verbindung

HRID 2182813

Reaktionsgleichung

Reaktionsgleichung von HRID 2182813
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:13]=[C:12]([OH:14])[NH:11][N:10]=1.S(OC)(O[CH3:19])(=O)=O.C(=O)([O-])[O-].[K+].[K+].N.Cl>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[CH:13]=[C:12]([OH:14])[N:11]([CH3:19])[N:10]=1

Komponenten

7

Edukt 5

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 6497Dimethyl SulfateHCID 11430Potassium CarbonateHCID 178515597HCID 178515597, Verbindung

Produkt 1

HCID 178481735HCID 178481735, VerbindungAusbeute 67,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

30 g of 3-(2,4-dichlorophenyl)-5-hydroxy-1H-pyrazole from Example 3.1 were initially charged in 750 ml of toluene. 23.1 g of dimethyl sulfate and 7.5 g of potassium carbonate were added, and the mixture was heated at reflux for 2 h. After cooling to room temperature, the mixture was made alkaline using ammonia and stirred overnight. The mixture was acidified by addition of hydrochloric acid (pH about 1) and cooled to room temperature, and the precipitated solid was filtered off. Drying gave 21.4 g of 3-(2,4-dichlorophenyl)-5-hydroxy-1-methyl-1H-pyrazole (purity according to GC 99.2%, yield 66.8%). M.p.: 128° C.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 2 h
  3. temperaturecooled to room temperature
  4. filtrationthe precipitated solid was filtered off
  5. customDrying

Quellen und Nachweise

ORD-Eintrag
ord-7699cd7ee4c345c598cec46a2ba68854
Quelldatensatz
uspto-grants-2005_05
Patentnummer
US06897322B2

Verknüpfte Notizen

Wird geladen…