反应详情

To 4-(6-fluoropyridin-3-yl)pyrrolidin-2-one (200 mg, 0.888 mmol) in DMF (4 mL) in ice bath was added NaH (42.6 mg, 1.066 mmol) and iodomethane (0.067 mL, 1.066 mmol). The reaction mixture was stirred in ice bath for 30 min and room temperature for 1 hour. LC-MS shows mixture of SM and product (1:1). Added again NaH (42.6 mg, 1.066 mmol) and iodomethane (0.067 mL, 1.066 mmol), stirred for 1 h at room temperature. Complete reaction by LC-MS. Reaction mixture was diluted with EtOAc and washed with water and bine. The organic layer was dried over sodium sulfate, filtered and evaporated. The crude was purified by flash chromatography [0-50-80% EtOAc (contains 10% MeOH)/heptane]. LCMS (m/z): 195.2 (MH+), 0.492 min. Yield 58%

1. waitroom temperature for 1 hour
2. additionmixture of SM and product (1:1)
3. stirringstirred for 1 h at room temperature
4. customreaction by LC-MS
5. customReaction mixture
6. washwashed with water and bine
7. dry with materialThe organic layer was dried over sodium sulfate
8. filtrationfiltered
9. customevaporated
10. customThe crude was purified by flash chromatography [0-50-80% EtOAc (contains 10% MeOH)/heptane]
11. custom195.2 (MH+), 0.492 min