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
Procedure
In a four-necked flask equipped with a stirrer, a thermometer and a condenser, 184.4 g (1.0 mol) of cyanuric chloride and 800 ml of acetonitrile were dissolved at room temperature, and a system was cooled, followed by adding dropwise 303.7 g (5.0 mol) of 28% aqueous ammonia over 2 hours while vigorously stirring and maintaining reaction temperature at not more than 10° C. After that, stirring was continued for 1 hour after heating to room temperature, followed by gradually heating to 50° C. and further aging for 4 hours. After cooling to room temperature, a product was filtered and washed with a large quantity of an ion-exchanged water, followed by drying in vacuo to obtain 115 g (yield of 79%) of 2,4-bis(amino)-6-chloro-1,3,5-triazine.
Workup
- customIn a four-necked flask equipped with a stirrer
- temperaturea system was cooled
- temperaturemaintaining
- customreaction temperature at not more than 10° C
- stirringAfter that, stirring
- temperatureby gradually heating to 50° C.
- waitfurther aging for 4 hours
- temperatureAfter cooling to room temperature
- filtrationa product was filtered
- washwashed with a large quantity of an ion-exchanged water
- customby drying in vacuo
Sources & evidence
- ORD record
- ord-5e5cf39ed3a24ae784053d18d9949ed7
- Source dataset
- uspto-grants-2000_09
- Patent number
- US06124381
Reaction notes
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