反应详情

温度

120 °C

3-Bromo-6-chloro-imidazo[1,2-b]pyridazine [13526-66-4] (1.1 g, 4.5 mmol) and piperazine [110-85-0] (3.6 g, 41.8 mmol) were ground together in a mortar to an intimate mixture and transferred to a 15 mL round bottomed flask containing a magnetic stir bar. The flask was fitted to a reflux condenser, N2 blanketed, and the reaction pot immersed in an ambient temperature oil bath. While the neat solid mixture stirred, the bath was heated to 120° C. over 0.5 h and held at nominal temperature for a total of 17 h. The bath was removed and the molten reaction allowed to cool and to solidify. The solid mass was dissolved in methanol, transferred to a separatory funnel, and partitioned between brine (pH adjusted to 10 with 3N aqueous sodium hydroxide) and ethyl acetate. The phase separated extract was dried (MgSO4) and evaporated to afford 0.9 g of 3-bromo-6-piperazin-1-yl-imidazo[1,2-b]pyridazine as a light yellow solid which was used without further purification. LRMS (ESI) m/z 282.1/284.1 [(M+H)]+, calc'd for C10H12BrN5: 282.14.

1. customtransferred to a 15 mL round bottomed flask
2. additioncontaining a magnetic stir bar
3. customThe flask was fitted to a reflux condenser
4. customthe reaction
5. custompot immersed in an ambient temperature
6. customheld at nominal temperature for a total of 17 h
7. customThe bath was removed
8. customthe molten reaction
9. temperatureto cool
10. customtransferred to a separatory funnel
11. custompartitioned between brine (
12. customThe phase separated
13. extractionextract
14. dry with materialwas dried (MgSO4)
15. customevaporated