HRID569193

反应详情

EQUATION

反应方程式

HRID 569193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

46.5 g (0.206 mole) of 2,4-bis-allylamino-6-chloro-1,3,5-triazine and 39.5 g (0.1 mole) of N,N'-bis-(2,2,6,6-tetramethylpiperid-4-yl)-hexamethylenediamine are dissolved rapidly by stirring in 200 ml of xylene in an atmosphere of nitrogen, a clear solution being formed initially. A precipitate of the hydrochlorides begins to form after approx. 10-15 minutes. The mixture is stirred for a further 2.5 hours at reflux temperature. A total of 8.8 g (0.22 mole) of finely powdered solid sodium hydroxide is then added in 5 portions in the course of 5 hours, and stirring is continued for a further 10 hours at reflux temperature. The reaction mixture is worked up by being filtered while hot (approx. 125°) through a preheated suction filter, the residue is washed with a little warm xylene, and the filtrate is induced to crystallise by stirring and cooling (0°-5°). The crystalline precipitate is filtered off and recrystallised from special boiling point gasoline (boiling point 110°-140°), which gives N,N'-bis-[2,4-di-(allylamino)-1,3,5-triazin-6-yl]-N,N'-bis-(2,2,6,6-tetramethylpiperid-4-yl)-hexamethylenediamine of melting point 161°-163°. This product is identical with the product prepared in accordance with Example 1b) (stabiliser No. 1).

WORKUP

后处理

  1. customa clear solution being formed initially
  2. customto form after approx. 10-15 minutes
  3. temperatureat reflux temperature
  4. stirringstirring
  5. waitis continued for a further 10 hours
  6. temperatureat reflux temperature
  7. filtrationby being filtered while hot (approx. 125°) through a preheated suction
  8. filtrationfilter
  9. washthe residue is washed with
  10. temperaturea little warm xylene
  11. customto crystallise
  12. stirringby stirring
  13. temperaturecooling (0°-5°)
  14. filtrationThe crystalline precipitate is filtered off
  15. customrecrystallised from special boiling point gasoline (boiling point 110°-140°), which