反应详情

温度

50 °C

10% Palladium on carbon (0.563 g, 0.53 mmol) and tert-butyl 4-(3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)piperazine-1-carboxylate (1.97 g, 5.29 mmol) were stirred in MeOH (30 mL) under an atmosphere of hydrogen at atmospheric temperature and pressure for 3 days. The catalyst was removed by filtration and the solvents evaporated. The residues were re-dissolved in MeOH (50 mL), 5% palladium on carbon (0.4 g, 0.09 mmol) was added and the mixture was stirred under an atmosphere of hydrogen at 50° C. and 5 Bar pressure until complete conversion was obtained. The catalyst was removed by filtration, washed with MeOH then DCM/MeOH and the solvent was evaporated to afford tert-butyl 4-(3-(trifluoromethyl)-7,8-dihydro-[1,2,4]triazolo[4,3-b]pyridazin-6-yl)piperazine-1-carboxylate (1.880 g, 9%) as a solid.

1. customThe catalyst was removed by filtration
2. customthe solvents evaporated
3. dissolutionThe residues were re-dissolved in MeOH (50 mL)
4. custom5 Bar pressure until complete conversion was obtained
5. customThe catalyst was removed by filtration
6. washwashed with MeOH
7. customDCM/MeOH and the solvent was evaporated