反应详情

温度

50 °C

To a stirring solution of 4-(3,5-dimethyl-[1,2,4]triazol-1-yl)-5-methyl-2H-pyrazol-3-ol (1 g, 5.18 mmol) (Intermediate A) in DMF (25 ml) was added Cs2CO3 (1.771 g, 5.43 mmol). The mixture was left to stir at 50° C. for 30 minutes and then treated with of 2-bromo-1-(4-methoxy-2-methyl-phenyl)-propan-1-one (Intermediate B) (1.397 g, 5.43 mmol) in DMF (10 ml). The mixture was stirred at 50° C. for 1 hour and concentrated in vacuo. The residue was dissolved in water (300 ml) and extracted with EtOAc (3×150 ml). The combined organic extracts were washed with NaHCO3, water, dried (MgSO4) and concentrated in vacuo to yield a pale yellow solid. Purification of the solid by chromatography on silica eluting with 20-100% EtOAc in iso-hexane afforded the title compound as a white solid; LC-MS Rt 1.03 mins; MS m/z 370.3 [M+H]+; Method 2minLC—30_v002.

1. waitThe mixture was left
2. stirringThe mixture was stirred at 50° C. for 1 hour
3. concentrationconcentrated in vacuo
4. dissolutionThe residue was dissolved in water (300 ml)
5. extractionextracted with EtOAc (3×150 ml)
6. washThe combined organic extracts were washed with NaHCO3, water
7. dry with materialdried (MgSO4)
8. concentrationconcentrated in vacuo
9. customto yield a pale yellow solid
10. customPurification of the solid by chromatography on silica eluting with 20-100% EtOAc in iso-hexane