Allylamine → HCID 20148735, Verbindung

HRID 569195Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 569195
[CH2:1]([NH2:4])[CH:2]=[CH2:3].[Cl:5][C:6]1[N:11]=[C:10](Cl)[N:9]=[C:8]([N:13]([CH:39]2[CH2:44][C:43]([CH3:46])([CH3:45])[NH:42][C:41]([CH3:48])([CH3:47])[CH2:40]2)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][N:20]([C:31]2[N:36]=[C:35]([Cl:37])[N:34]=[C:33](Cl)[N:32]=2)[CH:21]2[CH2:26][C:25]([CH3:28])([CH3:27])[NH:24][C:23]([CH3:30])([CH3:29])[CH2:22]2)[N:7]=1.[OH-].[Na+]>C1(C)C=CC=CC=1.O>[Cl:5][C:6]1[N:11]=[C:10]([NH:4][CH2:1][CH:2]=[CH2:3])[N:9]=[C:8]([N:13]([CH:39]2[CH2:40][C:41]([CH3:47])([CH3:48])[NH:42][C:43]([CH3:45])([CH3:46])[CH2:44]2)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][N:20]([C:31]2[N:36]=[C:35]([Cl:37])[N:34]=[C:33]([NH:4][CH2:1][CH:2]=[CH2:3])[N:32]=2)[CH:21]2[CH2:22][C:23]([CH3:29])([CH3:30])[NH:24][C:25]([CH3:28])([CH3:27])[CH2:26]2)[N:7]=1

Komponenten

6

Edukt 3

HCID 7853AllylamineHCID 14798Sodium HydroxideHCID 21468019HCID 21468019, Verbindung

Produkt 1

HCID 20148735HCID 20148735, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 1140TolueneLösungsmittel

Versuchsvorschrift

17.2 g (0.3 mole) of anhydrous allylamine are added dropwise, in the course of one hour, at 30°-40° and while stirring, to a solution of 103.6 g (0.15 mole) of N,N'-bis-(2,4-dichloro-1,3,5-triazin-6-yl)-N,N'-bis-(2,2,6,6-tetramethylpiperid-4-yl)-hexamethylenediamine in 500 ml of toluene. A solution of 12.0 g (0.3 mole) of sodium hydroxide in 100 ml of water is then added at approx. 30°, and stirring is continued for a further 19 hours at 50°. The mixture is worked up by separating off the aqueous phase in a separating funnel, washing the organic phase with three times 200 ml of water, drying it over sodium sulfate and removing the solvent by vacuum distillation. The solid residue is recrystallised from ethyl methyl ketone, which gives pure N,N'-bis-(2-chloro-4-allylamino-1,3,5-triazin-6-yl)-N,N'-bis-(2,2,6,6-tetramethylpiperid-4-yl)-hexamethylenediamine of melting point 210°-211°.

Aufarbeitung

  1. customby separating off the aqueous phase in a separating funnel
  2. washwashing the organic phase with three times 200 ml of water
  3. dry with materialdrying it over sodium sulfate
  4. customremoving the solvent
  5. distillationby vacuum distillation
  6. customThe solid residue is recrystallised from ethyl methyl ketone, which

Quellen und Nachweise

ORD-Eintrag
ord-46754e814ff042cca44c5ee8b035efcf
Quelldatensatz
uspto-grants-1988_03
Patentnummer
US04731393

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