反应详情

A stirred solution of 6-chloro-3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazine (4.44 g, 20.0 mmol), azetidin-3-ylmethanol (2.25 g, 22.0 mmol) and DIPEA (5.21 mL, 30.0 mmol) in DMF (40 mL) was heated at 70° C. for 1 hour. The solution was evaporated and partitioned between water and 2M aqueous K2CO3. The organic phase was washed with water and brine and dried over MgSO4. The crude product was purified by MPLC silica chromatography, eluting with 5% MeOH in DCM. Pure fractions were evaporated to dryness and triturated with ether, giving [1-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]azetidin-3-yl]methanol (1.65 g, 30%) as a cream crystalline solid.

1. customThe solution was evaporated
2. custompartitioned between water and 2M aqueous K2CO3
3. washThe organic phase was washed with water and brine
4. dry with materialdried over MgSO4
5. customThe crude product was purified by MPLC silica chromatography
6. washeluting with 5% MeOH in DCM
7. customPure fractions were evaporated to dryness
8. customtriturated with ether