Reaktion #311761

Reaktionsgleichung

potassium carbonate

2-cyanoethylhydrazine

acetonitrile

hydrogen chloride

hydrogen chloride

→

1-(2-cyanoethyl)-5-chloro-3-hydroxy-1,2,4-triazole

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigewere passed in at -10° C
2. 2
   Temperaturwhilst cooling
3. 3
   workup.ADDITIONwere added
4. 4
   workup.STIRRINGThis mixture was first stirred for 2 hours at room temperature
5. 5
   Temperaturwas then heated
6. 6
   Sonstige(5 to 6 hours)
7. 7
   TemperaturAfter cooling
8. 8
   Filtrationthe mixture was filtered
9. 9
   Waschenthe residue was washed with acetonitrile
10. 10
    Einengenthe entire filtrate was concentrated by evaporation in vacuo
11. 11
    Temperaturcooled to -10° to -15° C
12. 12
    SonstigeThe colorless crystals which had precipitated
13. 13
    Filtrationwere filtered off
14. 14
    Sonstigedried

Vorschrift

17 g (0.2 mole) of 2-cyanoethylhydrazine were dissolved in 100 ml of acetonitrile and 7.3 g of hydrogen chloride gas were passed in at -10° C. Thereafter, 32 g of N-chlorocarbonylisocyanide dichloride were added dropwise at 0° C., whilst cooling and stirring well, and after completion of this addition, 30 g of potassium carbonate were added. This mixture was first stirred for 2 hours at room temperature and was then heated under reflux until no further evolution of hydrogen chloride was detectable (5 to 6 hours). After cooling, the mixture was filtered, the residue was washed with acetonitrile and the entire filtrate was concentrated by evaporation in vacuo. The oil which remained was taken up in a little ethanol and cooled to -10° to -15° C. The colorless crystals which had precipitated were filtered off and dried. 20 g of 1-(2-cyanoethyl)-5-chloro-3-hydroxy-1,2,4-triazole of melting point 149°-150° C. were obtained. ##STR23##

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