反应详情

温度

2.5 °C

(810 mg, 3.0 mmol) 1-(6-Bromo-pyridin-3-yl)-4,4-dimethyl-imidazolidin-2-one (Example 3, step 1) was dissolved in DMF (8 ml) and cooled to 0-5° C. Iodomethane (640 mg, 280 μl, 4.5 mmol, 1.5 equiv.) and NaH (60%) (156 mg, 3.9 mmol, 1.3 equiv.) were added and the mixture was stirred for 2 hours at 0-5° C. The reaction mixture was treated with sat. NaHCO3 solution and extracted two times with EtOAc. The organic layers were extracted with water and brine, dried over Na2 SO4 and evaporated to dryness. The crude product was purified by flash chromatography on a silica gel column eluting with a heptane:ethyl acetate gradient 100:0 to 0:100. The desired 1-(6-bromo-pyridin-3-yl)-3,4,4-trimethyl-imidazolidin-2-one (800 mg, 94% yield) was obtained as a yellow solid, MS: m/e=284.1/286.0 (M+M+).

1. extractionextracted two times with EtOAc
2. extractionThe organic layers were extracted with water and brine
3. customdried over Na2 SO4
4. customevaporated to dryness
5. customThe crude product was purified by flash chromatography on a silica gel column
6. washeluting with a heptane