反应详情

温度

23 °C

To a solution of 1-methyl-3-phenyl-1H-1,2,4-triazole (310 mg, 1.95 mmol, see J. Chem. Soc., 1954, 3319-3322) in THF (25 mL) cooled to −78° C. was added 1.6 M n-butyl lithium (1.33 mL, 2.12 mmol) dropwise and stirred for 15 min. Next a solution of Intermediate 368.2 (500 mg, 1.77 mmol) in THF (5 mL) was added dropwise and stirred for 5 min before allowing the mixture to warm to 23° C. The mixture was quenched with aqueous NH4Cl and extracted with EtOAc (3×50 mL). The organic layer was washed with H2O, brine, dried (Na2SO4) and concentrated. The crude product was purified by flash chromatography (0 to 60% EtOAc/hexanes gradient) to afford 440 mg of Example 368.3. HPLC (2 min gradient) RT=2.42 min.

1. stirringstirred for 5 min
2. customThe mixture was quenched with aqueous NH4Cl
3. extractionextracted with EtOAc (3×50 mL)
4. washThe organic layer was washed with H2O, brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customThe crude product was purified by flash chromatography (0 to 60% EtOAc/hexanes gradient)