반응 #452890

반응 방정식

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

1,4-dioxane

octadecylamine

sodium hydroxide

→

titled compound

수율 91.0%

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

수율 91.0%

용매

water

water

반응 조건

후처리

1. 1
   온도was warmed
2. 2
   기타to react at a reflux temperature for 3 hours
3. 3
   기타to react for additional 2 hours
4. 4
   온도After 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
   추출to extract the product in the organic layer
8. 8
   세척After washing the organic layer with water sufficiently
9. 9
   workup.DISTILLATIONthe solvent was distilled off from the organic layer

실험 절차

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.

출처