Ammonia → 1,3,5-Triazine-2,4-diamine, 6-chloro-

HRID 610401Notes

Reaction equation

HRID 610401 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]=1

Participants

4

Conditions

Temperature
0 °C

Procedure

184.5 g (1.0 mol) of cyanuric chloride was dissolved in 800 mL of acetonitrile at room temperature, and 303.7 g (5.0 mol) of 28%-aqueous ammonia was added dropwise into the solution cooled to 0° C., over 2 hours while vigorously stirring and maintaining the reaction temperature at not more then 10° C. After the completion of dropwise addition, cooling was stopped, and stirring was continued for 1 hour at room temperature, followed by gradually heating to 45° C. and allowing to further react for 4 hours. After cooling, a product was filtered, followed by washing with a large quantity of water. The filtered product was dried at 50° C. in vacuo for 6 hours to obtain 115 g (a yield of 79%) of the above-identified compound.

Workup

  1. temperaturemaintaining the reaction temperature at not more then 10° C
  2. additionAfter the completion of dropwise addition
  3. temperaturecooling
  4. stirringstirring
  5. temperatureby gradually heating to 45° C.
  6. customto further react for 4 hours
  7. temperatureAfter cooling
  8. filtrationa product was filtered
  9. washby washing with a large quantity of water
  10. customThe filtered product was dried at 50° C. in vacuo for 6 hours
  11. customto obtain 115 g (a yield of 79%) of the above-identified compound

Sources & evidence

ORD record
ord-c7d92b3d395c4f6394a39ec098e973d0
Source dataset
uspto-grants-1999_12
Patent number
US05998573

Reaction notes

Loading…