تفاعل #80260

ord-44ea6459c73449988937bfaeef87df1a

معادلة التفاعل

CCN(CC)CC
triethylamine
Nc1cnccn1
3-aminopyrazine
S=C=S
carbon disulfide
CCOC(C)=O
ethyl acetate
CC[NH+](CC)CC.S=C([S-])Nc1cnccn1
triethylammonium N-(2-pyrazinyl)-dithiocarbamate
المردود 31.6%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05616456uspto-grants-1997_04