反应详情

6-Chloro-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine trifluoroacetate (W2.002b; 50 mg) was dissolved in ethanol (3.5 ml) while stirring at RT. Thereafter, sodium ethoxide was added dropwise while cooling with ice (25 mg dissolved in 1.5 ml of ethanol). After stirring at RT for 2.5 h, the mixture was heated to 60° C. and, after 2.5 h, a further equivalent of sodium ethoxide solution was added. After standing overnight, the mixture was heated again to 60° C., two further equivalents of sodium ethoxide solution were added and the mixture was stirred for 4 h. Subsequently, the mixture was admixed with water and 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. 27 mg of the title compound were obtained. LC-MS rt: 0.67 min [M+H]+: 194.1 (met. a)

1. stirringAfter stirring at RT for 2.5 h
2. temperaturethe mixture was heated to 60° C. and, after 2.5 h
3. temperaturethe mixture was heated again to 60° C.
4. stirringthe mixture was stirred for 4 h
5. extractionextracted three times with dichloromethane
6. dry with materialThe combined organic phases were dried over sodium sulfate
7. filtrationafter the desiccant had been filtered off
8. customdried under reduced pressure