N-(1,1-Dimethylethyl)benzenemethanamine → HCID 20458608, Verbindung

HRID 544751

Reaktionsgleichung

Reaktionsgleichung von HRID 544751
C(NC(OC1C=C(C(=O)C[Br:21])C=C(OC(=O)NCC)C=1)=O)C.[CH2:23]([NH:30][C:31]([CH3:34])([CH3:33])[CH3:32])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>CC(C)=O>[BrH:21].[CH2:23]([NH:30][C:31]([CH3:34])([CH3:33])[CH3:32])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

Komponenten

4

Edukt 2

HCID 76908N-(1,1-Dimethylethyl)benzenemethanamineHCID 20458601HCID 20458601, Verbindung

Produkt 1

HCID 20458608HCID 20458608, VerbindungAusbeute 78,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Versuchsvorschrift

To a solution of 8.0 g of 3',5'-bis-(N-ethylcarbamoyloxy)-2-bromo acetophenone in 100 ml of acetone was added 7.0 g of N-benzyl-t-butylamine. The mixture was refluxed for 18 hours. The 4.1 g of N-benzyl-t-butylamine hydrobromide formed and precipitated during the reaction was filtered off and the filtrate was acidified with conc. HCl. The filtrate was now evaporated to dryness and the title compound was isolated by column chromatography on Silica gel 60 using (1) CHCl3 /ethanol (2:1), (2) ethanol as eluants. The title compound was eluted in the ethanol fraction and recrystallized from ethanol/diethylether. The identity of the product was confirmed with NMR.

Aufarbeitung

  1. temperatureThe mixture was refluxed for 18 hours

Quellen und Nachweise

ORD-Eintrag
ord-7fe92459100740a0b008c2a568a04930
Quelldatensatz
uspto-grants-1984_05
Patentnummer
US04451663

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