反应详情

6-Chloro-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide (W2.001; 100 mg) were initially charged in water (1 ml) and admixed with piperidine (260 μl) with stirring. Thereafter, the mixture was heated to reflux for 1 h and, after cooling, freed of the solvent. Subsequently, the mixture was admixed with water and the solid formed was filtered off with suction and dried. The mother liquor was dried and admixed with a little water. The solid obtained was filtered off with suction and dried. The filtrate was then extracted three times with dichloromethane. The combined organic phases were dried over sodium sulfate and, after the desiccant had been filtered off, dried under reduced pressure. The three resulting solid fractions were combined and gave rise to 56 mg of the title compound.

1. temperatureThereafter, the mixture was heated
2. temperatureto reflux for 1 h
3. temperatureafter cooling, freed of the solvent
4. customthe solid formed
5. filtrationwas filtered off with suction
6. customdried
7. customThe mother liquor was dried
8. customThe solid obtained
9. filtrationwas filtered off with suction
10. customdried
11. extractionThe filtrate was then extracted three times with dichloromethane
12. dry with materialThe combined organic phases were dried over sodium sulfate
13. filtrationafter the desiccant had been filtered off
14. customdried under reduced pressure