Ethanol, reaction products with ammonia, distn. residues → HCID 54094556, Verbindung

HRID 1977985Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1977985
[CH3:1][O:2][C:3]1[CH:12]=[C:11]2[C:6]([CH2:7][CH2:8][CH2:9][C:10]2=[CH:13][C:14]#[N:15])=[CH:5][CH:4]=1.N.C(O)C>C(O)C.[Ni]>[NH2:15][CH2:14][CH:13]=[C:10]1[C:11]2[C:6](=[CH:5][CH:4]=[C:3]([O:2][CH3:1])[CH:12]=2)[CH2:7][CH2:8][CH2:9]1

Komponenten

5

Edukt 2

HCID 22020343Ethanol, reaction products with ammonia, distn. residuesHCID 54328648(E)-2-(7-methoxy-3,4-dihydronaphthalen-1(2H)-ylidene)acetonitrile

Produkt 1

HCID 54094556HCID 54094556, VerbindungAusbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 935NickelKatalysatorHCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

To a solution of (1,2,3,4-tetrahydro-7-methoxy-1-naphthylidene)acetonitrile (15.0 g, 25 mmol) in ethanol (100 ml) were added a saturated ammonia/ethanol solution (30 ml) and Raney nickel (W-2, 3 g). The reaction mixture was stirred for 8 hours at 50° C. under hydrogen atmosphere (3-4 kgf /cm2). The Raney nickel was filtered off, then the solvent was distilled off under reduced pressure to give the above-titled compound (a mixture of isomers (20.4 g, yield 80%, oil). This compound was used in the subsequent reaction without further purification.

Aufarbeitung

  1. filtrationThe Raney nickel was filtered off
  2. distillationthe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9ed2a8b2b3be43028dc7b94878229e42
Quelldatensatz
uspto-grants-2001_05
Patentnummer
US06235789B1

Notizen zur Reaktion

Wird geladen…