反应详情

A mixture of (S)-1-(6-chloro[1,2,4]triazolo[4,3-b]pyridazin-3-yl)ethanol (30.0 mg, 0.151 mmol), 1-methyl-4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyrazole (62.8 mg, 0.302 mmol), Pd(PPh3)4 (20 mg, 0.02 mmol), potassium carbonate (62.6 mg, 0.453 mmol) and 4:1 dioxane:water (5 mL) was heated to 85° C. for 1 h. The organic solvent was removed in vacuo, and the material was transferred to a separatory funnel and extracted with DCM. The organic layer was dry-loaded onto silica gel, and the material was purified via column chromatography, eluting with 10% MeOH/DCM. The fractions containing the pure product were concentrated in vacuo to afford the title compound as a white solid. MS (ES+): m/z 245.08 (100) [MH+]. HPLC: tR=2.00 min (ZQ3, polar—5 min).

1. customThe organic solvent was removed in vacuo
2. customthe material was transferred to a separatory funnel
3. extractionextracted with DCM
4. customthe material was purified via column chromatography
5. washeluting with 10% MeOH/DCM
6. additionThe fractions containing the pure product
7. concentrationwere concentrated in vacuo