反应详情

温度

50 °C

Cyclopropylmethanol (2.84 ml) was initially charged in DMF (20 ml), admixed under argon with sodium hydride (862 mg) and stirred at 50° C. for 1 h. Subsequently, 6-chloro-7,8-dimethyl-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide (W2.006, 2 g), dissolved in DMF (20 ml), and one equivalent of the alkoxide solution were 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. Then the reaction mixture was dried and purified using silica gel (40 g cartridge, dichloromethane/methanol gradient of 0-10% in 40 min). 625 mg of the title compound were obtained. LC-MS rt: 0.62 min [M+H]+: 234.1 (met. b)

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