2-Methylbenzoyl chloride → 1-Methyl-5-(o-tolyl)-3-phenyl-1,2,4-triazole

HRID 1111868Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1111868
Cl.[CH3:2][NH:3][NH:4][C:5](=[NH:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[C:13]1([CH3:22])[C:14]([C:19](Cl)=O)=[CH:15][CH:16]=[CH:17][CH:18]=1>C(OCC)C>[CH3:2][N:3]1[C:19]([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=2[CH3:22])=[N:12][C:5]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)=[N:4]1

Komponenten

4

Edukt 2

HCID 702762-Methylbenzoyl chlorideHCID 178486233HCID 178486233, Verbindung

Produkt 1

HCID 218245451-Methyl-5-(o-tolyl)-3-phenyl-1,2,4-triazoleAusbeute 76 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3283Diethyl EtherLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of 0.56 g. of benzimidic acid 2-methylhydrazide hydrochloride and 3.8 g. of o-toluic acid chloride is heated under stirring at about 120° C. After cooling and addition of diethyl ether, the hydrochloride of the triazole is collected on filter and then suspended in a sodium bicarbonate aqueous solution. The free base is extracted with diethyl ether and the organic phase, after drying over sodium sulfate, is evaporated. The crude compound is purified by distillation at 160° C/0.1 mm Hg. Yield 76%.

Aufarbeitung

  1. additionA mixture of 0.56 g
  2. temperatureAfter cooling
  3. customthe hydrochloride of the triazole is collected
  4. filtrationon filter
  5. extractionThe free base is extracted with diethyl ether
  6. dry with materialthe organic phase, after drying over sodium sulfate
  7. customis evaporated
  8. distillationThe crude compound is purified by distillation at 160° C/0.1 mm Hg

Quellen und Nachweise

ORD-Eintrag
ord-7fa73e849b2446649b87bcb0e40d9066
Quelldatensatz
uspto-grants-1978_10
Patentnummer
US04119635

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