反応 #80260

反応方程式

triethylamine

3-aminopyrazine

carbon disulfide

ethyl acetate

→

triethylammonium N-(2-pyrazinyl)-dithiocarbamate

収率 31.6%

溶媒

hexane

反応条件

後処理

1. 1
   workup.STIRRINGAfter the mixture was stirred at 60° C. for 5 hr
2. 2
   その他to precipitate yellow crystals
3. 3
   その他The crystals were separated from the solution by filtration
4. 4
   洗浄washed with 5 ml of ethyl acetate

実験手順

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).

出典