反应详情

温度

40 °C

1,3-Dimethoxypropan-2-ol (12.96 ml) was initially charged in DMF (25 ml), admixed under argon with sodium hydride (681 mg) and stirred at 40° C. for 1 h. Subsequently, 6-chloro-[1,2,4]triazolo[4,3-b]pyridazin-3-ylamine hydrobromide (W2.002; 1.5 g), dissolved in DMF (25 ml), was added dropwise within 20 min. After 1 h, the mixture was admixed with water and extracted by shaking four times with dichloromethane. The combined organic phases were dried over magnesium sulfate and concentrated by rotary evaporation. The residue was triturated with MtB ether, filtered off with suction and dried. 764 mg of the title compound were isolated. LC-MS rt: 0.74 min [M+H]+: 268.1 (met. a)

1. additionwas added dropwise within 20 min
2. waitAfter 1 h
3. extractionextracted
4. stirringby shaking four times with dichloromethane
5. dry with materialThe combined organic phases were dried over magnesium sulfate
6. concentrationconcentrated by rotary evaporation
7. customThe residue was triturated with MtB ether
8. filtrationfiltered off with suction
9. customdried