反应详情

温度

50 °C

To a solution of 1-(3-fluoro-4-methoxyphenyl)-N-methoxy-N-methyl-5-oxopyrrolidine-3-carboxamide (Step 1, 2 g, 6.75 mmol) in 30 mL of THF was added 2 M phenylmagnesium chloride in THF (6.75 mL) via syringe at RT. The solution was heated to 50° C. for 2 h. The solution was poured to 50 mL of satd. NH4Cl aq. soln. The resulting mixture was extracted with 100 mL of EtOAc. The organic phase was washed with 50 mL of brine, dried over Na2SO4 and concentrated in vacuo. The crude was purified by a silica gel column chromatography (10% to 80% EtOAc/hexane) to give white solid. MS (ESI pos. ion) m/z: 314.2 (M+H). Calc'd Exact Mass for C18H16FNO3: 313.32.

1. additionThe solution was poured to 50 mL of satd
2. extractionThe resulting mixture was extracted with 100 mL of EtOAc
3. washThe organic phase was washed with 50 mL of brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo
6. customThe crude was purified by a silica gel column chromatography (10% to 80% EtOAc/hexane)
7. customto give white solid