Reaktion #80260

Reaktionsgleichung

triethylamine

3-aminopyrazine

carbon disulfide

ethyl acetate

→

triethylammonium N-(2-pyrazinyl)-dithiocarbamate

Ausbeute 31.6%

Lösungsmittel

hexane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGAfter the mixture was stirred at 60° C. for 5 hr
2. 2
   Sonstigeto precipitate yellow crystals
3. 3
   SonstigeThe crystals were separated from the solution by filtration
4. 4
   Waschenwashed with 5 ml of ethyl acetate

Vorschrift

In a 100-ml flask, 4.9 g (50 mmol) of 3-aminopyrazine, 4.5 g (59 mmol) of carbon disulfide and 50 ml of ethyl acetate were placed, and 6.5 g (64 mmol) of triethylamine was added dropwise with stirring over a 5-min period on a water bath. After the mixture was stirred at 60° C. for 5 hr. 10 ml of hexane was added to the mixture, which was allowed to stand overnight at room temperature to precipitate yellow crystals. The crystals were separated from the solution by filtration, and washed with 5 ml of ethyl acetate to obtain 4.3 g of triethylammonium N-(2-pyrazinyl)-dithiocarbamate (Intermediate II-1). Yield 31%. Mp 113°-116° C. (dec).

Quelle