Water → HCID 14746198, compound

HRID 484942Notes

Reaction equation

HRID 484942 reaction equation
[N:1]1[C:8](Cl)=[N:7][C:5](Cl)=[N:4][C:2]=1[Cl:3].[CH3:10][C:11]1([CH3:21])[CH2:16][CH:15]([NH:17][CH3:18])[CH2:14][C:13]([CH3:20])([CH3:19])[NH:12]1.C(=O)([O-])[O-].[K+].[K+].O>C1(C)C(C)=CC=CC=1>[Cl:3][C:2]1[N:1]=[C:8]([N:17]([CH3:18])[CH:15]2[CH2:14][C:13]([CH3:20])([CH3:19])[NH:12][C:11]([CH3:21])([CH3:10])[CH2:16]2)[N:7]=[C:5]([N:17]([CH:15]2[CH2:14][C:13]([CH3:20])([CH3:19])[NH:12][C:11]([CH3:21])([CH3:10])[CH2:16]2)[CH3:18])[N:4]=1

Participants

6

Reactant 4

HCID 962WaterHCID 7954Cyanuric chlorideHCID 11430Potassium CarbonateHCID 13657792N,2,2,6,6-Pentamethylpiperidin-4-amine

Product 1

HCID 14746198HCID 14746198, compound

Reagents, catalysts & solvents 1

HCID 7237O-XyleneSolvent

Procedure

18.4 g of cyanuric chloride and 34.0 g of 2,2,6,6-tetramethyl-4-(methylamino)piperidine were dissolved in 250 ml of xylene, and the solution was stirred at a temperature of 90°-110° C. for 3 hours. 30 ml of a saturated aqueous solution of potassium carbonate were then added and the resulting mixture was heated under reflux for 5 hours. At the end of this time, the reaction mixture was poured into water and extracted with benzene. The extract was dried over anhydrous potassium carbonate and then the benzene was distilled off. The residue was recrystallized from ethyl acetate, giving the title compound in the form of crystals melting at 179°-180° C.

Workup

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 5 hours
  3. extractionextracted with benzene
  4. dry with materialThe extract was dried over anhydrous potassium carbonate
  5. distillationthe benzene was distilled off
  6. customThe residue was recrystallized from ethyl acetate

Sources & evidence

ORD record
ord-661d6bf82301429b8477411ae58d6a7c
Source dataset
uspto-grants-1985_08
Patent number
US04533688

Reaction notes

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