反应详情

4-(5-{[3-(trifluoromethyl)phenyl]amino}-4H-1,2,4-triazol-3-yl)phenol (160 mg, 0.5 mmol) was dissolved in 3 mL of anhydrous dioxane in 2-5 mL microwave vial (Personal Chemistry). Solid Cs2CO3 (163.0 mg, 0.5 mmol) was added, followed by 4-chloro-2,6,-diaminopyrimidine (79.5 mg, 0.55 mmol). The vial was capped and microwaved at 200° C. for 20 min. Then ca. 3 mL of MeOH was added to dissolve the formed suspension, the solution was transferred into a round-bottom flask and solvent was removed in vacuo. The residue was re-dissolved in 3 mL of DMF, filtered through 0.22 u syringe filter and purified by reverse phase preparative HPLC using acetonitrile/water system with 0.01% of TFA.

1. customThe vial was capped
2. custommicrowaved at 200° C. for 20 min
3. dissolutionto dissolve the formed suspension
4. customthe solution was transferred into a round-bottom flask
5. customsolvent was removed in vacuo
6. dissolutionThe residue was re-dissolved in 3 mL of DMF
7. filtrationfiltered through 0.22 u syringe
8. filtrationfilter
9. custompurified by reverse phase preparative HPLC