反应详情

温度

70 °C

A mixture of 4-(6-aminomethylpyridin-2-yl)-2-(diaminomethyleneamino)thiazole trihydrochloride (1.7 g), triethylamine (2.0 ml) and 1,1-bis(methylthio)-2-nitroethylene (0.9 g) was stirred at 70° C. for 7 hours. After cooling to ambient temperature, to the mixture was added a 40% aqueous methylamine (2.5 ml) and the mixture was stirred at ambient temperature for 15 hours. The reaction mixture was added to water, and the isolated precipitate was collected by filtration and dried. 4N-Dioxanoic hydrogen chloride (2.2 ml) was added to a mixture of above resulting precipitate in methanol (9.0 ml) and the mixture was stirred at ambient temperature for 1 hour. To the mixture was added a diisopropyl ether (9.0 ml) and the isolated precipitate was collected by filtration. The precipitate was recrystallized from an aqueous ethanol to give 2-(diaminomethyleneamino)-4-[6-[N-(1-methylamino-2-nitrovinyl)aminomethyl]pyridin-2-yl]thiazole (0.47 g).

1. temperatureAfter cooling to ambient temperature, to the mixture
2. stirringthe mixture was stirred at ambient temperature for 15 hours
3. filtrationthe isolated precipitate was collected by filtration
4. customdried
5. addition4N-Dioxanoic hydrogen chloride (2.2 ml) was added to a mixture of above resulting precipitate in methanol (9.0 ml)
6. stirringthe mixture was stirred at ambient temperature for 1 hour
7. additionTo the mixture was added a diisopropyl ether (9.0 ml)
8. filtrationthe isolated precipitate was collected by filtration
9. customThe precipitate was recrystallized from an aqueous ethanol