反应详情

To a solution of 1-(4-(6,7-dimethoxyquinolin-4-yloxy)-3-fluorophenyl)-4-(hydroxy(phenyl)methyl)pyrrolidin-2-one (Example 48, 0.1 g, 0.2 mmol) in THF/DMF (1 mL:1 mL) was added NaH (0.1 g, 2.5 mmol) solid. The reaction was stirred at RT for 1 h. MeI (0.1 mL, 1.6 mmol) was added via a syringe and the reaction was stirred for 1 h. The reaction was quenched with 10 mL of satd. NH4Cl solution and 10 mL of water. The solution was diluted with 50 mL of EtOAc. The organic phase was separated and was washed with 30 mL of brine, dried over Na2SO4 and concentrated in vacuo. The crude oil was purified by chromatography (10% EtOAc/hexanes to EtOAc) to give colorless film. MS (ESI pos. ion) m/z: 503.5 (M+H). Calc'd Exact Mass for C29H27FN2O5: 502.53.

1. stirringthe reaction was stirred for 1 h
2. customThe reaction was quenched with 10 mL of satd
3. additionThe solution was diluted with 50 mL of EtOAc
4. customThe organic phase was separated
5. washwas washed with 30 mL of brine
6. dry with materialdried over Na2SO4
7. concentrationconcentrated in vacuo
8. customThe crude oil was purified by chromatography (10% EtOAc/hexanes to EtOAc)
9. customto give colorless film