HRID345998

反应详情

EQUATION

反应方程式

HRID 345998 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.3 g of diethanolamine and a solution of 1 g of NaOH in 3 ml of water are added to a solution of 20 g of 2-chloro-4-morpholino-6-(4,4-ethylenedioxy-2,2,6,6-tetramethylpiperidin-1-yl)-1,3,5-triazine (product from Example 44) in 50 ml of xylene. 1 g of NaOH in 3 ml of water is again added after 1.75 hours with stirring under reflux. After 14 hours, 7.9 g of diethanolamine are added, after which the mixture is stirred under reflux for a further 28 hours. It is then allowed to cool and washed with water, and the organic phase is separated off. After drying over Na2SO4, evaporating and recrystallizing twice from toluene, the above product is obtained as a white powder which melts at 135°-140°.

WORKUP

后处理

  1. temperatureunder reflux
  2. stirringafter which the mixture is stirred
  3. temperatureunder reflux for a further 28 hours
  4. temperatureto cool
  5. washwashed with water
  6. customthe organic phase is separated off
  7. dry with materialAfter drying over Na2SO4
  8. customevaporating
  9. customrecrystallizing twice from toluene
  10. customthe above product is obtained as a white powder which melts at 135°-140°