Cyanuric chloride → 2-Chloro-4,6-bis(2,2,6,6-tetramethyl-4-piperidylamino)-1,3,5-triazine

HRID 26975

Reaktionsgleichung

Reaktionsgleichung von HRID 26975
[CH3:1][C:2]1([CH3:11])[CH2:7][CH:6]([NH2:8])[CH2:5][C:4]([CH3:10])([CH3:9])[NH:3]1.C(=O)([O-])[O-].[Na+].[Na+].[N:18]1[C:25](Cl)=[N:24][C:22](Cl)=[N:21][C:19]=1[Cl:20]>CC(C)=O.O>[Cl:20][C:19]1[N:18]=[C:25]([NH:8][CH:6]2[CH2:5][C:4]([CH3:10])([CH3:9])[NH:3][C:2]([CH3:11])([CH3:1])[CH2:7]2)[N:24]=[C:22]([NH:8][CH:6]2[CH2:7][C:2]([CH3:11])([CH3:1])[NH:3][C:4]([CH3:10])([CH3:9])[CH2:5]2)[N:21]=1

Komponenten

6

Edukt 3

HCID 7954Cyanuric chlorideHCID 10340Sodium CarbonateHCID 375244-Amino-2,2,6,6-tetramethylpiperidine

Produkt 1

HCID 214680172-Chloro-4,6-bis(2,2,6,6-tetramethyl-4-piperidylamino)-1,3,5-triazine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 180AcetoneLösungsmittel2×HCID 962WaterLösungsmittel

Versuchsvorschrift

62.4 g of 2,2,6,6-tetramethyl-4-amino-piperidine in 200 ml of acetone and, at the same time, 42.4 g of sodium carbonate dissolved in 100 ml of water are added to a finely dispersed suspension of cyanuric chloride, prepared by adding 36.9 g of the latter in 200 ml of boiling acetone to 400 ml of ice water. The temperature is kept at 0°-5° C. by means of external cooling. After the addition is complete, the reaction mixture is allowed slowly to warm to room temperature and is stirred at this temperature for 3 hours. Filtering and recrystallisation of the product from ethyl acetate/hexane gives 46.3 g of a white crystalline product, melting point 270° C.

Aufarbeitung

  1. customprepared
  2. customis kept at 0°-5° C. by means of external cooling
  3. additionAfter the addition
  4. filtrationFiltering
  5. customrecrystallisation of the product from ethyl acetate/hexane

Quellen und Nachweise

ORD-Eintrag
ord-b7218be49b3d482993418ba5ee590b49
Quelldatensatz
uspto-grants-1979_04
Patentnummer
US04151356

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