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

HRID 904663

Reaktionsgleichung

Reaktionsgleichung von HRID 904663
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 204586013',5'-bis-(N-ethylcarbamoyloxy)-2-bromo acetophenone

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-2c26adbca5da4cac866dbebb3bdc88d7
Quelldatensatz
uspto-grants-1983_12
Patentnummer
US04419364

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