Ethanol → HCID 19816098, Verbindung

HRID 2247861Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2247861
[N+:1]([C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[N:10]1[CH2:19][CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11]1)([O-])=O.C([OH:22])C>O=[Pt]=O>[NH2:1][C:4]1[CH:9]=[CH:8][N:7]=[CH:6][C:5]=1[N+:10]1([O-:22])[CH2:19][CH2:18][C:17]2[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=2)[CH2:11]1

Komponenten

4

Edukt 2

HCID 702EthanolHCID 198160942-(4-Nitropyridin-3-yl)-1,2,3,4-tetrahydroisoquinoline

Produkt 1

HCID 19816098HCID 19816098, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 345198Adams' catalystKatalysator

Versuchsvorschrift

To a slurry of PtO2 (0.3 g) in 10 ml of ethanolwas added 2-(4-nitro-3-pyridinyl)-1,2,3,4-tetrahydroisoquinoline, N-oxide (5.0 g) in 240 ml of ethanol and this was hydrogenated with a Parr apparatus at room temperature for 24 hours. The mixture was filtered and the filtrate concentrated to yield an oil (5.1 g), which was eluted with 20% methanol/DCM on a silica gel column via HPLC. The desired fractions were concentrated to a solid (2.0 g), m.p. 216°-219° C. (decomp). This solid was recrystallized from acetonitrile to yield a solid, 1.0 g, m.p. 217°-219° C.

Aufarbeitung

  1. filtrationThe mixture was filtered
  2. concentrationthe filtrate concentrated

Quellen und Nachweise

ORD-Eintrag
ord-f5cfdaf0e8134d20bc4e187d0ce9a61f
Quelldatensatz
uspto-grants-1991_08
Patentnummer
US05037835

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