HRID1744763
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
6.00 g (42.9 mmol) 5,6-dimethyluracil was dissolved in 26 mL of hexamethyldisilazane and 2.1 mL DMF. The mixture was heated for 11 hours at 150° C. and the excess of hexamethyldisilazane was removed under reduced pressure. Toluene was added to the mixture and evaporated off under reduced pressure to remove any residual hexamethyldisilazane. The residue was dissolved in 25 mL of iodomethane, refluxed for 2 hours, the excess iodomethane then evaporated off under reduced pressure and the residue recrystallized from deionised water yielding after drying 5.76 g (87%) of 1,5,6-trimethyluracil (m.p. 254–257° C., lit. 256–258° C.).
WORKUP
后处理
- customthe excess of hexamethyldisilazane was removed under reduced pressure
- additionToluene was added to the mixture
- customevaporated off under reduced pressure
- customto remove any residual hexamethyldisilazane
- dissolutionThe residue was dissolved in 25 mL of iodomethane
- temperaturerefluxed for 2 hours
- customthe excess iodomethane then evaporated off under reduced pressure
- customthe residue recrystallized from deionised water yielding
- dry with materialafter drying 5.76 g (87%) of 1,5,6-trimethyluracil (m.p. 254–257° C., lit. 256–258° C.)