Aluminium lithium hydride → 2-[(4-Chlorophenyl)methyl]azepane

HRID 27437

Reaktionsgleichung

Reaktionsgleichung von HRID 27437
[H-].[Al+3].[Li+].[H-].[H-].[H-].[Cl:7][C:8]1[CH:22]=[CH:21][C:11]([CH2:12][CH:13]2[NH:19][C:18](=O)[CH2:17][CH2:16][CH2:15][CH2:14]2)=[CH:10][CH:9]=1>O1CCCC1>[Cl:7][C:8]1[CH:22]=[CH:21][C:11]([CH2:12][CH:13]2[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][NH:19]2)=[CH:10][CH:9]=1

Komponenten

4

Edukt 2

HCID 21226445Aluminium lithium hydrideHCID 233428517-(4-Chlorobenzyl)perhydroazepin-2-one

Produkt 1

HCID 39338092-[(4-Chlorophenyl)methyl]azepaneAusbeute 68,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Add 0.5 g of lithium aluminum hydride to a solution of 2.8 g 7-(4-chlorobenzyl)-perhydroazepin -2-one in 30 ml of tetrahydrofurane. Boil the mixture under reflux for 16 hours, cool it and then carefully treat it with ice-water. After extraction with diethyl ether, dry the extract over sodium sulfate concentrate the oily residue and distill in a vacuum to obtain 1.8 g of the title compound with a BP of 90° to 92° at 0.05 mm Hg.

Aufarbeitung

  1. temperatureBoil the mixture under reflux for 16 hours
  2. temperaturecool it
  3. extractionAfter extraction with diethyl ether
  4. customdry the
  5. extractionextract over sodium sulfate
  6. concentrationconcentrate the oily residue
  7. distillationdistill in a vacuum

Quellen und Nachweise

ORD-Eintrag
ord-32cc92d9280349b984ea48408cc67dba
Quelldatensatz
uspto-grants-1980_09
Patentnummer
US04221788

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