反应详情

A mixture 4-chloro-5-ethoxycarbonylmethyl-2-(2-methylprop-2-yl)pyrimidine (18 g), toluene (180 cm3), zinc dust (36 g) and 3 molar ammonium hydroxide solution saturated with sodium chloride (180 cm3) was heated at 100° C. for 120 hours. After cooling and filtering to remove the solid component the organic phase was separated, the aqueous phase washed with ethyl acetate and the washings combined with the organic phase. After washing the organic phase with water and drying over anhydrous magnesium sulphate the solvents were removed by evaporation under reduced pressure and the residual oil (16 g) was subjected to purification by column chromatography using a silica column eluted with dichloromethane to yield 5-ethoxycarbonylmethyl-2-(2-methylprop-2-yl)pyrimidine (12 g) as a yellow oil.

1. temperatureAfter cooling
2. filtrationfiltering
3. customto remove the solid component the organic phase
4. customwas separated
5. washthe aqueous phase washed with ethyl acetate
6. washAfter washing the organic phase with water
7. dry with materialdrying over anhydrous magnesium sulphate the solvents
8. customwere removed by evaporation under reduced pressure
9. customthe residual oil (16 g) was subjected to purification by column chromatography
10. washeluted with dichloromethane