反应详情

4-(5-{[3-(trifluoromethyl)phenyl]amino}-4H-1,2,4-triazol-3-yl)phenol (100 mg, 0.31 mmol) was dissolved in 3 mL of anhydrous dioxane in 2-5 mL microwave vial (Personal Chemistry). Solid Cs2CO3 (101.7 mg, 0.31 mmol) was added, followed by 4-amino-6-chloro-2-(methylthio)-pyrimidine (60.3 mg, 0.34 mmol). The vial was capped and microwaved at 200° C. for 10 min. Then ca. 3 mL of MeOH was added to dissolve the formed suspension. The resulting reddish-brown 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. The fractions, containing the product, were collected and partitioned between EtOAc and saturated aqueous NaHCO3. Ethyl acetate layer was washed with brine, dried over anhydrous sodium sulfate and filtered. Solvent was removed in vacuo to give the title compound as a white solid (39.5 mg).

1. customThe vial was capped
2. custommicrowaved at 200° C. for 10 min
3. dissolutionto dissolve the formed suspension
4. customThe resulting reddish-brown 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
10. additionThe fractions, containing the product
11. customwere collected
12. custompartitioned between EtOAc and saturated aqueous NaHCO3
13. washEthyl acetate layer was washed with brine
14. dry with materialdried over anhydrous sodium sulfate
15. filtrationfiltered
16. customSolvent was removed in vacuo