반응 #80260

반응 방정식

triethylamine

3-aminopyrazine

carbon disulfide

ethyl acetate

→

triethylammonium N-(2-pyrazinyl)-dithiocarbamate

수율 31.6%

용매

hexane

반응 조건

후처리

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

실험 절차

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).

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