反应详情

Lithium diethylamide (2M solution in THF) (3.92 mL, 7.84 mmol) was added to a solution of 2-(2-oxo-piperidin-1-yl)-phenol (as described in Example 1, Step F) (0.50 g, 2.61 mmol) in THF (5 mL) at −78° C. with stirring under Ar. After 30 min, iodomethane (0.488 mL, 7.84 mmol) was added and the reaction left to come to room temperature overnight. The reaction was treated with H2O, concentrated to remove the THF, then partitioned between diethyl ether and H2O. The organic layer was separated, washed with brine, dried (Na2SO4), filtered, and concentrated to dryness to give the title compound after chromatography (silica gel, 1% CH3OH, 29% EtOAc, 70% hexane).

1. waitthe reaction left
2. waitto come to room temperature overnight
3. concentrationconcentrated
4. customto remove the THF
5. custompartitioned between diethyl ether and H2O
6. customThe organic layer was separated
7. washwashed with brine
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated to dryness