反应详情

温度

0 °C

To a solution of 4-cyclobutyl-5-(5-methoxy-4H-1,2,4-triazol-3-yl)-2-methylbenzamide (compound 89.8, 0.1 g, 0.33 mmol) in TFA (5 mL) at 0° C., was added NaNO2 (46 mg, 0.66 mmol). The mixture was stirred at 0° C. for 1 hour, then at room temperature for 2 hours. The mixture was concentrated under reduced pressure and the residue was partitioned between EtOAc and brine. The aqueous layer was extracted with EtOAc and the combined organic layers were dried (Na2SO4), filtered and concentrated under reduced pressure to yield 0.1 g (theoretical) of the title compound as a clear oil. m/z (ES+) 288 (M+H)+.

1. waitat room temperature for 2 hours
2. concentrationThe mixture was concentrated under reduced pressure
3. customthe residue was partitioned between EtOAc and brine
4. extractionThe aqueous layer was extracted with EtOAc
5. dry with materialthe combined organic layers were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure