HRID269797
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
1.2 g, 6 mmol, of 6-methyl-1,3-dipropyl-1,3-dihydropyrimidine-2,4-dione, as prepared in Example 1, was added in small portions to a cooled (0° C.) solution of concentrated sulfuric acid (3.0 ml) and nitric acid (2.0 ml). The reaction stirred at 0° C. for 2 hours. The reaction mixture was poured over ice and a green amorphous solid formed. The solid was removed by filtration and washed copiously with water. The solid was dissolved in dichloromethane and concentrated. The residue was purified using column chromatography (1:1.2 EtOAc:Hexanes) to yield 6-methyl-5-nitro-1,3-dipropyl-1,3-dihydropyrimidine-2,4-dione(0.430 g, HNMR)
WORKUP
后处理
- additionwas added in small portions to
- additionThe reaction mixture was poured over ice
- customa green amorphous solid formed
- customThe solid was removed by filtration
- washwashed copiously with water
- dissolutionThe solid was dissolved in dichloromethane
- concentrationconcentrated
- customThe residue was purified