反应详情

温度

95 °C

To a solution of N,N′ Dipropyl urea (10.0 g, 69.4 mmol) in pyridine (60 ml) was added acetic anhydride (21.6 ml, 229 mmol) and 4-(dimethylamino)pyridine (8.5 g, 69.4 mmol). The mixture was heated to 95° C. for 1.5 hours. The reaction mixture was cooled and the solvent was removed under vacuum. The residue was then dissolved in dichloromethane (200 ml) and washed with 2N HCl (2×60 ml) and saturated sodium bicarbonate (2×60 ml). The organic layer was concetrated and purified using column chromatography (2:1 Hexane:Ethyl Acetate) to yield 6-methyl-1,3-dipropyl-1,3-dihydropyrimidine-2,4-dione(4.0 g, M+1=210.92)

1. temperatureThe reaction mixture was cooled
2. customthe solvent was removed under vacuum
3. dissolutionThe residue was then dissolved in dichloromethane (200 ml)
4. washwashed with 2N HCl (2×60 ml) and saturated sodium bicarbonate (2×60 ml)
5. custompurified