HRID129468

反应详情

EQUATION

反应方程式

HRID 129468 的结构方程式

PROCEDURE

实验过程

8 ml of 25% oleum are added dropwise with cooling at a maximum of 10° C. to 8 ml of 100% nitric acid. 12.4 g (0.10 mol) of 4-hydroxy-6-ethylpyrimidine are then introduced in portions at a maximum of 35° C. The temperature is kept at 40° C. overnight. For the purpose of reacting further any starting material that remains, a further 13 ml of 25% oleum and 11 ml of 100% nitric acid are added dropwise at a maximum of 40° C. The mixture is left for 12 hours at 40° C. to complete the reaction and is then poured carefully onto ice and extracted completely with ethyl acetate, and the extracts are washed with sodium hydrogen carbonate solution. The extract is concentrated using a rotary evaporator, whereupon 11.8 g (69.7% of the theoretical yield) of pure substance crystallise out; m.p. 181°-183° C.

WORKUP

后处理

  1. waitThe mixture is left for 12 hours at 40° C.
  2. customthe reaction
  3. additionis then poured carefully onto ice
  4. extractionextracted completely with ethyl acetate
  5. washthe extracts are washed with sodium hydrogen carbonate solution
  6. concentrationThe extract is concentrated
  7. customa rotary evaporator
  8. customwhereupon 11.8 g (69.7% of the theoretical yield) of pure substance
  9. customcrystallise out