Nitrogen → HCID 14833063, compound

HRID 2372551Notes

Reaction equation

HRID 2372551 reaction equation
N#N.C([O-])(O)=O.[Na+].[NH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.[N:14]1[C:21](Cl)=[N:20][C:18](Cl)=[N:17][C:15]=1Cl.[NH:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1.C([O-])([O-])=O.[Na+].[Na+]>O>[N:8]1([C:15]2[N:17]=[C:18]([N:8]3[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]3)[N:20]=[C:21]([N:23]3[CH2:28][CH2:27][N:26]([C:15]4[N:17]=[C:18]([N:8]5[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]5)[N:20]=[C:21]([N:8]5[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]5)[N:14]=4)[CH2:25][CH2:24]3)[N:14]=2)[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1

Participants

8

Reactant 6

HCID 947NitrogenHCID 4837PiperazineHCID 7954Cyanuric chlorideHCID 8082PiperidineHCID 10340Sodium CarbonateHCID 516892Sodium Bicarbonate

Product 1

HCID 14833063HCID 14833063, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Conditions

Temperature
20 °C

Procedure

All operations are carried out under a blanket of N2. 1 mol of each of NaHCO3 and piperidine are introduced into 0.8 1 of water, and 0.5 mol of cyanuric chloride is added in portions at room temperature sufficiently slowly that the reaction temperature is 20° C. and the pH is between 7 and 11. The reaction mixture is subsequently stirred at 20° C. for a further 100 minutes and refluxed for 30 minutes. After cooling, 0.25 mol of each of piperazine and Na2CO3 as 13% strength by weight and 20% strength by weight aqueous solutions respectively are added simultaneously, and the mixture is stirred at room temperature for a further 2 hours and refluxed for 17 hours. The resultant suspension is filtered with suction, washed with water and the residue is dried to constant weight. A finely crystalline, white powder is obtained.

Workup

  1. additionis added in portions at room temperature sufficiently slowly that the reaction temperature
  2. customis 20° C.
  3. temperaturerefluxed for 30 minutes
  4. temperatureAfter cooling
  5. stirringthe mixture is stirred at room temperature for a further 2 hours
  6. temperaturerefluxed for 17 hours
  7. filtrationThe resultant suspension is filtered with suction
  8. washwashed with water
  9. customthe residue is dried to constant weight
  10. customA finely crystalline, white powder is obtained

Sources & evidence

ORD record
ord-163097b72aa341b7a97c9f1ff0fde0a5
Source dataset
uspto-grants-1992_03
Patent number
US05099017

Reaction notes

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