Sodium Hydroxide → TK 12997

HRID 569193

Reaktionsgleichung

Reaktionsgleichung von HRID 569193
[CH2:1]([NH:4][C:5]1[N:10]=[C:9]([NH:11][CH2:12][CH:13]=[CH2:14])[N:8]=[C:7](Cl)[N:6]=1)[CH:2]=[CH2:3].[CH3:16][C:17]1([CH3:43])[CH2:22][CH:21]([NH:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][NH:30][CH:31]2[CH2:36][C:35]([CH3:38])([CH3:37])[NH:34][C:33]([CH3:40])([CH3:39])[CH2:32]2)[CH2:20][C:19]([CH3:42])([CH3:41])[NH:18]1.[OH-].[Na+]>C1(C)C(C)=CC=CC=1>[CH2:1]([NH:4][C:5]1[N:10]=[C:9]([NH:11][CH2:12][CH:13]=[CH2:14])[N:8]=[C:7]([N:23]([CH:21]2[CH2:22][C:17]([CH3:43])([CH3:16])[NH:18][C:19]([CH3:42])([CH3:41])[CH2:20]2)[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH2:29][N:30]([C:7]2[N:8]=[C:9]([NH:11][CH2:12][CH:13]=[CH2:14])[N:10]=[C:5]([NH:4][CH2:1][CH:2]=[CH2:3])[N:6]=2)[CH:31]2[CH2:32][C:33]([CH3:40])([CH3:39])[NH:34][C:35]([CH3:38])([CH3:37])[CH2:36]2)[N:6]=1)[CH:2]=[CH2:3]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 27306N,N'-Diallyl-6-chloro-1,3,5-triazine-2,4-diamineHCID 934191,6-Bis(2,2,6,6-tetramethyl-4-piperidylamino)hexane

Produkt 1

HCID 163462TK 12997

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

46.5 g (0.206 mole) of 2,4-bis-allylamino-6-chloro-1,3,5-triazine and 39.5 g (0.1 mole) of N,N'-bis-(2,2,6,6-tetramethylpiperid-4-yl)-hexamethylenediamine are dissolved rapidly by stirring in 200 ml of xylene in an atmosphere of nitrogen, a clear solution being formed initially. A precipitate of the hydrochlorides begins to form after approx. 10-15 minutes. The mixture is stirred for a further 2.5 hours at reflux temperature. A total of 8.8 g (0.22 mole) of finely powdered solid sodium hydroxide is then added in 5 portions in the course of 5 hours, and stirring is continued for a further 10 hours at reflux temperature. The reaction mixture is worked up by being filtered while hot (approx. 125°) through a preheated suction filter, the residue is washed with a little warm xylene, and the filtrate is induced to crystallise by stirring and cooling (0°-5°). The crystalline precipitate is filtered off and recrystallised from special boiling point gasoline (boiling point 110°-140°), which gives N,N'-bis-[2,4-di-(allylamino)-1,3,5-triazin-6-yl]-N,N'-bis-(2,2,6,6-tetramethylpiperid-4-yl)-hexamethylenediamine of melting point 161°-163°. This product is identical with the product prepared in accordance with Example 1b) (stabiliser No. 1).

Aufarbeitung

  1. customa clear solution being formed initially
  2. customto form after approx. 10-15 minutes
  3. temperatureat reflux temperature
  4. stirringstirring
  5. waitis continued for a further 10 hours
  6. temperatureat reflux temperature
  7. filtrationby being filtered while hot (approx. 125°) through a preheated suction
  8. filtrationfilter
  9. washthe residue is washed with
  10. temperaturea little warm xylene
  11. customto crystallise
  12. stirringby stirring
  13. temperaturecooling (0°-5°)
  14. filtrationThe crystalline precipitate is filtered off
  15. customrecrystallised from special boiling point gasoline (boiling point 110°-140°), which

Quellen und Nachweise

ORD-Eintrag
ord-c3406a3fd78a4635813ec5eae250c075
Quelldatensatz
uspto-grants-1988_03
Patentnummer
US04731393

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