HCID 13136924, Verbindung → HCID 13136926, Verbindung

HRID 851198Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 851198
[CH3:1][C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][C:5]2[C:11]3[CH2:16][CH2:15][NH:14][CH2:13][C:12]=3[C:17](=[O:19])[O:18][C:4]=2[CH:3]=1.[H][H]>CN(C)C=O.CO.[Ni]>[NH2:8][C:7]1[C:2]([CH3:1])=[CH:3][C:4]2[O:18][C:17](=[O:19])[C:12]3[CH2:13][NH:14][CH2:15][CH2:16][C:11]=3[C:5]=2[CH:6]=1

Komponenten

6

Edukt 2

HCID 13136924HCID 13136924, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 13136926HCID 13136926, VerbindungAusbeute 81,2 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 935NickelKatalysator2×HCID 887MethanolLösungsmittelHCID 6228DimethylformamideLösungsmittel2×

Versuchsvorschrift

A solution of 1,2,3,4-tetrahydro-8-methyl-9-nitro-5H-[1]benzopyrano[3,4-c]pyridin-5-one (6.0 g, 0.023 moles) in N,N-dimethylformamide (100 ml) and methanol (50 ml) is hydrogenated at 50 psi in the presence of Raney Nickel (0.5 g) at room temperature for 20 hours. Additional Raney Nickel (0.5 g) in N,N-dimethylformamide (50 ml) is then added, and hydrogenation resumed until hydrogen uptake ceases. The catalyst is filtered off and rinsed with warm N,N-dimethylformamide. The filtrate is concentrated under reduced pressure and filtered to afford the product (4.3 g), mp 283°-284° C.

Aufarbeitung

  1. filtrationThe catalyst is filtered off
  2. washrinsed with warm N,N-dimethylformamide
  3. concentrationThe filtrate is concentrated under reduced pressure
  4. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-48376c66ea3949c982275571ed8d9c8c
Quelldatensatz
uspto-grants-1983_05
Patentnummer
US04382939

Notizen zur Reaktion

Wird geladen…