Réaction #96226

Équation de réaction

cyanuric chloride

3-(diethylamino)propylamine

potassium carbonate

→

2-chloro-4,6-bis[3-(diethylamino)propyl]amino-1,3,5-triazine

Solvants

water

Conditions de réaction

Traitement

1. 1
   Températurewhile maintaining 3°-5° C. by means of an external ice-water bath
2. 2
   Températurewhile maintaining 3°-12° C. by means of an ice-water bath
3. 3
   workup.WAITto stand overnight
4. 4
   AutreThe solid which precipitated
5. 5
   Filtrationwas collected by filtration
6. 6
   workup.DISSOLUTIONdissolved by the addition of hydrochloric acid
7. 7
   workup.ADDITIONSlowly 10 percent aqueous potassium carbonate was added until the mixture
8. 8
   FiltrationThe resulting solid was collected by filtration
9. 9
   Lavagewashed with water
10. 10
    Autredried in vacuo

Mode opératoire

Following the procedure described in Japanese Pat. No. 39272/74, 50.0 ml of water was cooled to 3° C. and slowly 18.4 g (0.1 mole) of cyanuric chloride was added while maintaining 3°-5° C. by means of an external ice-water bath. Slowly 26.0 g (0.2 mole) of 3-(diethylamino)propylamine was added while maintaining 3°-12° C. by means of an ice-water bath. The resulting solution was stirred at ambient temperature for approximately eight hours and allowed to stand overnight. Slowly a 10 percent aqueous potassium carbonate solution was added to the reaction solution until it was slightly alkaline. The solid which precipitated was collected by filtration. The water wet filter cake was resuspended in water and dissolved by the addition of hydrochloric acid. Slowly 10 percent aqueous potassium carbonate was added until the mixture was slightly alkaline. The resulting solid was collected by filtration, washed with water and dried in vacuo to obtain 2-chloro-4,6-bis[3-(diethylamino)propyl]amino-1,3,5-triazine, a water-insoluble, white colored solid which melted at 119° C.

Source