反应详情

温度

50 °C

LiH (7.7 mg, 0.97 mmol) was added to the solution of methyl 2-oxo-1,2-dihydropyridine-3-carboxylate (0.10 g, 0.65 mmol) in DMF (3 mL) at 0° C. After stirring for 30 minutes, (bromomethyl) cyclopropane (0.18 g, 1.30 mmol) was added to the reaction mixture at the temperature, and the reaction was warmed to 50° C. After stirring for 3 days at 50° C., the reaction mixture was diluted with EtOAc, quenched with ice water, extracted with EtOAc, dried over MgSO4, and concentrated. The crude was purified by silica gel flash column chromatography (2% MeOH in CH2Cl2) to afford 87 mg (64%) of the desired product.

1. stirringAfter stirring for 3 days at 50° C.
2. customquenched with ice water
3. extractionextracted with EtOAc
4. dry with materialdried over MgSO4
5. concentrationconcentrated
6. customThe crude was purified by silica gel flash column chromatography (2% MeOH in CH2Cl2)