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