反应详情

温度

50 °C

Cyclopropylmethanol (2.99 ml) was initially charged in DMF (30 ml), admixed under argon with sodium hydride (907 mg) and stirred at 50° C. for 1 h. Subsequently, 6-chloro-8-methyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide (W2.002; 2.0 g) were dissolved in DMF (30 ml) and one equivalent of the alkoxide solution was added. After stirring at 50° C. for one hour, two further equivalents of alkoxide solution were added and the mixture was stirred further at 50° C. The reaction mixture was then dried and purified using silica gel (80 g cartridge, dichloromethane/methanol gradient of 0-10% in 40 min). 620 mg of the title compound were obtained. LC-MS rt: 0.57 min [M+H]+: 220.1 (met. b)

1. stirringAfter stirring at 50° C. for one hour
2. stirringthe mixture was stirred further at 50° C
3. customThe reaction mixture was then dried
4. custompurified
5. customsilica gel (80 g cartridge, dichloromethane/methanol gradient of 0-10% in 40 min)