反应详情

Triethylamine (1 ml) was added to a solution of 2-aminopropiophenone hydrochloride (0.93 g) and dimethyl cyanodithioimidocarbonate (0.73 g) in methanol (3 ml), and the mixture was refluxed for 15 minutes and evaporated under reduced pressure. The residue was dissolved in chloroform and the solution was washed with water, dried over sodium sulfate and concentrated under reduced pressure. The residue was dissolved in a small amount of ethyl acetate and diluted with diisopropyl ether. The resultant precipitates were collected by filtration, washed with diisopropyl ether and dried to give 2-(3-cyano-2-methyl-1-isothioureido)propiophenone (0.99 g).

1. temperaturethe mixture was refluxed for 15 minutes
2. customevaporated under reduced pressure
3. dissolutionThe residue was dissolved in chloroform
4. washthe solution was washed with water
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated under reduced pressure
7. dissolutionThe residue was dissolved in a small amount of ethyl acetate
8. additiondiluted with diisopropyl ether
9. customThe resultant precipitates
10. filtrationwere collected by filtration
11. washwashed with diisopropyl ether
12. customdried