HCID 5156493, Verbindung → HCID 10559687, Verbindung

HRID 968491Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 968491
Cl[C:2]1[C:11]([N+:12]([O-:14])=[O:13])=[CH:10][C:9]2[CH2:8][CH2:7][CH2:6][CH2:5][C:4]=2[N:3]=1.[NH3:15].CO>>[N+:12]([C:11]1[C:2]([NH2:15])=[N:3][C:4]2[CH2:5][CH2:6][CH2:7][CH2:8][C:9]=2[CH:10]=1)([O-:14])=[O:13]

Komponenten

3

Edukt 2

HCID 5156493HCID 5156493, VerbindungHCID 21705897Ammonia methanol

Produkt 1

HCID 10559687HCID 10559687, Verbindung

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of intermediate (9) (0.0658 mol) in NH3/CH3OH 7N (60 ml) was stirred at 120° C. for 12 hours in an autoclave. The solvent was evaporated till dryness. The residue was taken up in 2-propanone. The precipitate was filtered off and dried, yielding 8.6 g 5,6,7,8-tetrahydro-3-nitro-2-quinolinamine (intermediate 10). d) A mixture of intermediate (10) (0.031 mol) in methanol (100 ml) was hydrogenated at room temperature under a 3.105 Pa (3 bar) pressure for 30 minutes in a Parr apparatus. After uptake of hydrogen (3 equivalents), the catalyst was filtered through celite, rinced with methanol and the filtrate was evaporated till dryness. The product was used with further purification, yielding 5.07 g 5,6,7,8-tetrahydro-2,3-quinolinediamine (intermediate 11).

Aufarbeitung

  1. customThe solvent was evaporated till dryness
  2. filtrationThe precipitate was filtered off
  3. customdried

Quellen und Nachweise

ORD-Eintrag
ord-3eacdbdeca0a4819ad0f2cb810565eeb
Quelldatensatz
uspto-grants-2007_12
Patentnummer
US07304052B2

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