Реакция #452890

Уравнение реакции

2,4-diamino-6-chloro-1,3,5-triazine

1,4-dioxane

octadecylamine

sodium hydroxide

→

titled compound

Выход 91.0%

2,4-diamino-6-octadecylamino-1,3,5-triazine

Выход 91.0%

Растворители

water

water

Условия реакции

Обработка

1. 1
   Температураwas warmed
2. 2
   Другоеto react at a reflux temperature for 3 hours
3. 3
   Другоеto react for additional 2 hours
4. 4
   ТемператураAfter cooling the reaction mixture
5. 5
   workup.DISTILLATIONthe solvent was distilled off under reduced pressure, and 100 mL of water and 100 mL of toluene
6. 6
   workup.ADDITIONwere added
7. 7
   Экстракцияto extract the product in the organic layer
8. 8
   ПромывкаAfter washing the organic layer with water sufficiently
9. 9
   workup.DISTILLATIONthe solvent was distilled off from the organic layer

Методика

A mixed solution of 14.5 g (0.1 mol) of 2,4-diamino-6-chloro-1,3,5-triazine prepared in Reference Example 1, 60 mL of water, 60 mL of 1,4-dioxane, and 26.9 g (0.1 mol) of octadecylamine was warmed with stirring and allowed to react at a reflux temperature for 3 hours. Further, an aqueous solution of 4.0 g (0.1 mol) of sodium hydroxide in 20 mL of water was dropwise added thereto over 1 hour and the mixture was allowed to react for additional 2 hours. After cooling the reaction mixture, the solvent was distilled off under reduced pressure, and 100 mL of water and 100 mL of toluene were added to extract the product in the organic layer. After washing the organic layer with water sufficiently, the solvent was distilled off from the organic layer to obtain 34.4 g (yield 91%) of the titled compound. Melting point: 91° C.

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