Ethyl Acetate → 2-Amino-10,11-dihydro-dibenz[b,f]oxepin-10-one

HRID 437816Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 437816
[N+:1]([C:4]1[CH:19]=[CH:18][C:7]2[O:8][C:9]3[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=3[C:11](=[O:13])[CH2:12][C:6]=2[CH:5]=1)([O-])=O.C(OCC)(=O)C>[Pt]=O.C(O)C>[NH2:1][C:4]1[CH:19]=[CH:18][C:7]2[O:8][C:9]3[CH:17]=[CH:16][CH:15]=[CH:14][C:10]=3[C:11](=[O:13])[CH2:12][C:6]=2[CH:5]=1

Komponenten

5

Edukt 2

HCID 8857Ethyl AcetateHCID 2276785510,11-Dihydro-2-nitro-dibenz[b,f]oxepin-10-one

Produkt 1

HCID 227679272-Amino-10,11-dihydro-dibenz[b,f]oxepin-10-one

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 82844Platinum oxide (PtO)KatalysatorHCID 702EthanolLösungsmittel

Versuchsvorschrift

52.5 G. of 10,11-dihydro-2-nitro-dibenz[b,f]oxepin-10-one are suspended in 900 ml. of ethyl acetate and 450 ml. of ethanol and hydrogenated in the presence of 300 mg. of platinum oxide at room temperature and normal pressure. The catalyst is removed by filtration, the filtrate evaporated in vacuo. The residue is crystallized from benzene/hexane, and there is obtained 2-amino-10,11-dihydro-dibenz[b,f]oxepin-10-one having a melting point of 116°-117° C.

Aufarbeitung

  1. customat room temperature
  2. customThe catalyst is removed by filtration
  3. customthe filtrate evaporated in vacuo
  4. customThe residue is crystallized from benzene/hexane

Quellen und Nachweise

ORD-Eintrag
ord-2ea753e49db14aa782e102370bf193cf
Quelldatensatz
uspto-grants-1977_06
Patentnummer
US04032525

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