反应 #80260

反应方程式

triethylamine

3-aminopyrazine

carbon disulfide

ethyl acetate

→

triethylammonium N-(2-pyrazinyl)-dithiocarbamate

收率 31.6%

溶剂

hexane

反应条件

后处理

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

实验过程

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).

来源