HRID1744763

反应详情

EQUATION

反应方程式

HRID 1744763 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customthe excess of hexamethyldisilazane was removed under reduced pressure
  2. additionToluene was added to the mixture
  3. customevaporated off under reduced pressure
  4. customto remove any residual hexamethyldisilazane
  5. dissolutionThe residue was dissolved in 25 mL of iodomethane
  6. temperaturerefluxed for 2 hours
  7. customthe excess iodomethane then evaporated off under reduced pressure
  8. customthe residue recrystallized from deionised water yielding
  9. dry with materialafter drying 5.76 g (87%) of 1,5,6-trimethyluracil (m.p. 254–257° C., lit. 256–258° C.)