hexahydro-7-[(4-nitrophenyl)methyl]-2H-azepin-2-one → HCID 23342835, Verbindung

HRID 27438

Reaktionsgleichung

Reaktionsgleichung von HRID 27438
[N+:1]([C:4]1[CH:18]=[CH:17][C:7]([CH2:8][CH:9]2[NH:15][C:14](=O)[CH2:13][CH2:12][CH2:11][CH2:10]2)=[CH:6][CH:5]=1)([O-])=O>C(O)C.[Pt].[H][H]>[NH2:1][C:4]1[CH:18]=[CH:17][C:7]([CH2:8][CH:9]2[CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][NH:15]2)=[CH:6][CH:5]=1

Komponenten

4

Edukt 1

HCID 11970558hexahydro-7-[(4-nitrophenyl)methyl]-2H-azepin-2-one

Produkt 1

HCID 23342835HCID 23342835, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178506450HCID 178506450, VerbindungKatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

Hydrogenate 3.72 of 7-(4-nitrobenzyl)perhydroazepin-2-one in 50 mls of ethyl alcohol with platinum/hydrogen. After the absorption of hydrogen has ceased, filter off the catalyst and concentrate the filtrate. Dissolve the thus obtained 7-(4-aminobenzyl)-perhydroazepin-2-one in tetrahydrofuran. Add 680 mg of lithium aluminum hydride and boil the mixture under reflux. After cooling, treat it with ice-water and extract it with diethyl Dry the organic phase over sodium sulphate and concentrate it to obtain 2.0 g of the brown oily title compound.

Aufarbeitung

  1. customAfter the absorption of hydrogen
  2. filtrationfilter off the catalyst
  3. concentrationconcentrate the filtrate
  4. dissolutionDissolve the thus obtained 7-(4-aminobenzyl)-perhydroazepin-2-one in tetrahydrofuran
  5. additionAdd 680 mg of lithium aluminum hydride and boil the mixture
  6. temperatureunder reflux
  7. temperatureAfter cooling
  8. additiontreat it with ice-water
  9. extractionextract it with diethyl
  10. dry with materialDry the organic phase over sodium sulphate
  11. concentrationconcentrate it

Quellen und Nachweise

ORD-Eintrag
ord-216ecf3061c4435bb488641f80fd0567
Quelldatensatz
uspto-grants-1980_09
Patentnummer
US04221788

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