反应详情

tert-butyl 4-[4-(1-hydroxy-1H-pyrrolo[3,2-b]pyridin-6-yl)-1H-pyrazol-1-yl]piperidine-1-carboxylate (30 mg, 0.078 mmol, 1.0 eq), 1-(bromomethyl)-2-(trifluoromethyl)benzene (0.066 mmol), and K2CO3 (30 mg) in 1.5 ml of DMF were shaken at r.t. for 30 min and then filtered and evaporated. The resulting crude product was dissolved in 1.5 ml of methanol and 0.5 ml of 4.0 M HCl/dioxane was dropped in. The reaction was shaken at room temperature for 0.5-1 h. The solvent was evaporated and the residue was dissolved in 2 ml of DCM. To this solution were added 20 mg of NaHCO3, 10 mg of Na2CO3, and drops of water. After stirred for 10 min, the organic solution was separated and purified with preparation HPLC to give the final product.

1. filtrationfiltered
2. customevaporated
3. dissolutionThe resulting crude product was dissolved in 1.5 ml of methanol
4. addition0.5 ml of 4.0 M HCl/dioxane was dropped in
5. customThe solvent was evaporated
6. dissolutionthe residue was dissolved in 2 ml of DCM
7. additionTo this solution were added 20 mg of NaHCO3, 10 mg of Na2CO3, and drops of water
8. stirringAfter stirred for 10 min
9. customthe organic solution was separated
10. custompurified with preparation HPLC