HCID 21456038, Verbindung → HCID 21481150, Verbindung

HRID 435705Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 435705
[N+:1]([C:4]1[CH:32]=[CH:31][C:7]2[S:8][C:9]3[CH:30]=[CH:29][CH:28]=[CH:27][C:10]=3[CH:11]([N:13]3[CH2:18][CH2:17][N:16]([CH2:19][CH2:20][N:21]4[CH2:25][CH2:24][O:23][C:22]4=[O:26])[CH2:15][CH2:14]3)[CH2:12][C:6]=2[CH:5]=1)([O-])=O.[H][H]>C(OCC)(=O)C.[Pd]>[NH2:1][C:4]1[CH:32]=[CH:31][C:7]2[S:8][C:9]3[CH:30]=[CH:29][CH:28]=[CH:27][C:10]=3[CH:11]([N:13]3[CH2:14][CH2:15][N:16]([CH2:19][CH2:20][N:21]4[CH2:25][CH2:24][O:23][C:22]4=[O:26])[CH2:17][CH2:18]3)[CH2:12][C:6]=2[CH:5]=1

Komponenten

5

Edukt 2

HCID 21456038HCID 21456038, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 21481150HCID 21481150, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

24.1 g of 3-[ 2-[4-(10,11-dihydro-2-nitro-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl ]-2-oxazolidinone in 2000 ml of ethyl acetate are hydrogenated in the presence of 5.7 g of palladium/carbon (5%) at 70° C and 10 atmospheres of hydrogen. After filtration, the filtrate is concentrated under reduced pressure. There is obtained 3-[ 2-[4-(2-amino-10,11-dihydro-dibenzo[b,f]thiepin-10-yl)-1-piperazinyl]-ethyl ]-2-oxazolidinone which melts at 193°-196° C. After chromatographic purification over aluminium oxide using acetone/hexane as the elution agent, there is obtained a pure product which melts at 195.5°-196.5° C.

Aufarbeitung

  1. filtrationAfter filtration
  2. concentrationthe filtrate is concentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-16c5c4906ad64cb08bd98d0d2ffd8991
Quelldatensatz
uspto-grants-1977_02
Patentnummer
US04006144

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