반응 #96226

반응 방정식

cyanuric chloride

3-(diethylamino)propylamine

potassium carbonate

→

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

용매

water

반응 조건

후처리

1. 1
   온도while maintaining 3°-5° C. by means of an external ice-water bath
2. 2
   온도while maintaining 3°-12° C. by means of an ice-water bath
3. 3
   workup.WAITto stand overnight
4. 4
   기타The solid which precipitated
5. 5
   여과was 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
   여과The resulting solid was collected by filtration
9. 9
   세척washed with water
10. 10
    기타dried in vacuo

실험 절차

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.

출처