Cyanuric chloride → 6-chloro-2-N,4-N-bis[3-(diethylamino)propyl]-1,3,5-triazine-2,4-diamine

HRID 67948

Reaktionsgleichung

Reaktionsgleichung von HRID 67948
[N:1]1[C:8](Cl)=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].[CH2:10]([N:12]([CH2:17][CH3:18])[CH2:13][CH2:14][CH2:15][NH2:16])[CH3:11].C(=O)([O-])[O-].[K+].[K+]>O>[Cl:3][C:2]1[N:1]=[C:8]([NH:16][CH2:15][CH2:14][CH2:13][N:12]([CH2:17][CH3:18])[CH2:10][CH3:11])[N:7]=[C:5]([NH:16][CH2:15][CH2:14][CH2:13][N:12]([CH2:17][CH3:18])[CH2:10][CH3:11])[N:4]=1

Komponenten

5

Edukt 3

HCID 7954Cyanuric chlorideHCID 11430Potassium CarbonateHCID 61011N,N-Diethyl-1,3-propanediamine

Produkt 1

HCID 1159956-chloro-2-N,4-N-bis[3-(diethylamino)propyl]-1,3,5-triazine-2,4-diamine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  1. temperaturewhile maintaining 3°-5° C. by means of an external ice-water bath
  2. temperaturewhile maintaining 3°-12° C. by means of an ice-water bath
  3. waitto stand overnight
  4. customThe solid which precipitated
  5. filtrationwas collected by filtration
  6. dissolutiondissolved by the addition of hydrochloric acid
  7. additionSlowly 10 percent aqueous potassium carbonate was added until the mixture
  8. filtrationThe resulting solid was collected by filtration
  9. washwashed with water
  10. customdried in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-061bb215f0834c9395df7ca6efa3a061
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04347352

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