Sodium Hydroxide → N,N'-diheptyl-p-xylylenediamine

HRID 1770049Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1770049
[CH2:1]([NH:8][C:9](=O)[C:10]1[CH:25]=[CH:24][C:13]([C:14]([NH:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23])=O)=[CH:12][CH:11]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].[H-].COCCO[Al+]OCCOC.[OH-].[Na+]>C1(C)C=CC=CC=1>[CH2:17]([NH:16][CH2:14][C:13]1[CH:12]=[CH:11][C:10]([CH2:9][NH:8][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH3:7])=[CH:25][CH:24]=1)[CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH3:23]

Komponenten

5

Edukt 3

HCID 14798Sodium HydroxideHCID 4098298N,N'-diheptylterephthalamideHCID 22591236HCID 22591236, Verbindung

Produkt 1

HCID 14801556N,N'-diheptyl-p-xylylenediamineAusbeute 97,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

To a mixture of 3.6 g N,N'-diheptylterephthalamide obtained in Example 1 and 60 ml toluene, was added dropwise 15.6 ml of a 70% solution of bis(2-methoxyethoxy)aluminum hydride in toluene. After heating under reflux for three hours, the reaction mixture was treated with 30 ml of 2.5N aqueous caustic soda solution under ice cooling, and the toluene layer separated was washed with saturated aqueous solution of sodium chloride and dried over a drying agent. Distilling off the solvent from the dried solution gave 3.24 g of N,N'-diheptyl-p-xylylenediamine.

Aufarbeitung

  1. temperatureAfter heating
  2. temperatureunder reflux for three hours
  3. customthe toluene layer separated
  4. washwas washed with saturated aqueous solution of sodium chloride
  5. customdried over a drying agent
  6. distillationDistilling off the solvent from the dried solution

Quellen und Nachweise

ORD-Eintrag
ord-b59ae24b340c4160b73bb2f15813942f
Quelldatensatz
uspto-grants-1995_01
Patentnummer
US05384425

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