反应详情

温度

40 °C

Pyrimidine 61 (Example 43, 5.0 g, 14.1 mmol) is dissolved in dimethylacetamide/water (1:1) with sodium ascorbate (2.85 g, 14.4 mmol). Dihydroxyacetone dimer (2.57 g, 14.3 mmol) is added and the reaction mixture is heated to 40° C. while air is bubbled into the reaction mixture. After 4 h the reaction mixture is poured into 250 mL of H2O, and the formed solid collected by filtration. This solid is redissolved in CH2Cl2/MeOH (3:1, 500 mL), and dried over MgSO4. The crude product is adsorbed on SiO2 and purified by flash column chromatography using CH2Cl2/MeOH (20:1).

1. customis bubbled into the reaction mixture
2. additionAfter 4 h the reaction mixture is poured into 250 mL of H2O
3. filtrationthe formed solid collected by filtration
4. dissolutionThis solid is redissolved in CH2Cl2/MeOH (3:1, 500 mL)
5. dry with materialdried over MgSO4
6. custompurified by flash column chromatography