反应详情

Sodium hydride (50% w/w dispersion in oil; 0.57 g.) was added to ethanol (10 ml.) portionwise. To the resulting solution was added 3-aminopropanethiol hydrochloride (0.75 g.) and the mixture stirred at room temperature. 2-[2-(2,2,2-Trifluoroethyl)guanidino]6-chloropyrazine (0.5 g.) was added in one portion and the mixture heated under reflux on the steam bath overnight. The mixture was cooled, evaporated, water (10 ml.) added and the mixture extracted with ethyl acetate. The extracts were dried over magnesium sulphate, filtered and evaporated to yield an oil, which was chromatographed eluting with methanol/methylene chloride/ammonia 10:40:1 v/v/v to yield 2-[2-(2,2,2-trifluoroethyl)guanidino]-6-(3-aminopropylthio)pyrazine as a pale yellow solid (0.39 g.) which was used without further purification.

1. temperaturethe mixture heated
2. temperatureunder reflux on the steam bath overnight
3. temperatureThe mixture was cooled
4. customevaporated
5. additionwater (10 ml.) added
6. extractionthe mixture extracted with ethyl acetate
7. dry with materialThe extracts were dried over magnesium sulphate
8. filtrationfiltered
9. customevaporated
10. customto yield an oil, which
11. customwas chromatographed
12. washeluting with methanol/methylene chloride/ammonia 10:40:1 v/v/v