Ammonia → 1,3,5-Triazine-2,4-diamine, 6-chloro-
Reaction equation
[N:1]1[C:8]([Cl:9])=[N:7][C:5](Cl)=[N:4]C=1Cl.[NH3:10].[C:11](#[N:13])C>>[NH2:10][C:5]1[N:4]=[C:11]([NH2:13])[N:1]=[C:8]([Cl:9])[N:7]=1Participants
4
Conditions
- Temperature
- 0 °C
Procedure
To a solution of 184.5 g (1.0 mol) of cyanuric chloride dissolved in 800 ml of acetonitrile at room temperature and cooled to 0° C., 303.7 g (5.0) of 28% aqueous ammonia solution was added at dropwise over 2 hour with vigorous stirring such that the reaction temperature was maintained below 10° C. After completion of the addition, the cooling was stopped and the mixture was stirred at room temperature for 1 hour and then the temperature was gradually elevated to 45° C. and the reaction was continued for additional 4 hours. After cooling, the product was filtered off and further washed with a large amount of water. The filtrate was dried at 50° C. for 6 hours under vacuum to obtain 115 g (yield: 79%) of the titled compound.
Workup
- temperaturewas maintained below 10° C
- additionAfter completion of the addition
- stirringthe mixture was stirred at room temperature for 1 hour
- customwas gradually elevated to 45° C.
- temperatureAfter cooling
- filtrationthe product was filtered off
- washfurther washed with a large amount of water
- customThe filtrate was dried at 50° C. for 6 hours under vacuum
Sources & evidence
- ORD record
- ord-5ae7f8bbb99044b682c90bb2af40fbf4
- Source dataset
- uspto-grants-2001_10
- Patent number
- US06307046B1
Reaction notes
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