反应详情

温度

70 °C

A mixture of tert-butyl piperazine-1-carboxylate (8.29 g, 44.5 mmol) and ethanol (90 mL) was added to a mixture of DIPEA (9.16 mL, 52.6 mmol) and 6-chloro-3-(trifluoromethyl)-[1,2,4]triazolo[3,4-f]pyridazine (obtained as described in Monatsh. Chem. (1972) 103(6), 1591-603) (9.0 g, 40.4 mmol) in ethanol (90 mL). The mixture was heated at 70° C. for 11 hours and then allowed to cool to ambient temperature to give a precipitate. The is precipitate was collected by filtration, washed with chilled ethanol and then with water, and dried under vacuum to afford tert-butyl 4-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperazine-1-carboxylate (13.64 g, 90.6%) as a white solid that was used without further purification.

1. temperatureto cool to ambient temperature
2. customto give a precipitate
3. filtrationThe is precipitate was collected by filtration
4. washwashed with chilled ethanol
5. dry with materialwith water, and dried under vacuum