反应详情

温度

80 °C

4-[5-(4-chloro-3-trifluoromethyl-phenylamino)-4H [1,2,4]triazol-3-yl]-phenol (120.0 mg, 0.338 mmol) was dissolved in 3 mL of anhydrous DMF in a 5 mL microwave vial (Personal Chemistry). Solid potassium bis(trimethylsilyl)amide (81.0 mg, 0.406 mmol) was added and the reaction mixture was stirred with heating at 80° C. for 15 min, then 3-amino-6-chloro-pyridazine (48.2 mg, 0.372 mmol) was added, followed by anhydrous K2CO3 (46.7 mg, 0.338 mmol). Then the vial was capped and microwaved at 200° C. for 30 min. After reaction was complete, the reaction mixture was diluted with ca. 1 mL of MeOH, filtered through 0.22 um syringe filter and purified by reverse-phase preparative HPLC in acetonitrile/water system with 0.01% TFA. The product was isolated as a TFA salt (18.2 mg).

1. customThen the vial was capped
2. custommicrowaved at 200° C. for 30 min
3. customAfter reaction
4. filtrationfiltered through 0.22 um syringe
5. filtrationfilter
6. custompurified by reverse-phase preparative HPLC in acetonitrile/water system with 0.01% TFA