HCID 14010268, Verbindung → HCID 19863758, Verbindung

HRID 1381938Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1381938
[ClH:1].[CH:2](=[N:9][CH2:10][CH2:11][NH:12][S:13]([N:16]([CH3:18])[CH3:17])(=[O:15])=[O:14])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[H][H]>CO.[Pd]>[ClH:1].[CH2:2]([NH:9][CH2:10][CH2:11][NH:12][S:13]([N:16]([CH3:18])[CH3:17])(=[O:15])=[O:14])[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1

Komponenten

5

Edukt 2

HCID 14010268HCID 14010268, VerbindungHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 19863758HCID 19863758, VerbindungAusbeute 92,8 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A solution of 3.0 g (0.011 mole) of N-benzylidene-2-[N'-[(dimethylamino)sulfonyl]amino]ethylamine hydrochloride in 100 ml of methanol was hydrogenated, at 40 psi, over 0.3 g of 10% Pd-C catalyst until hydrogen uptake ceased (20 min.). The mixture was filtered and concentrated under reduced pressure to provide 3.0 g of crude product. The NMR spectrun was consistent with the assigned structure and the crude product was utilized directly without further purification.

Aufarbeitung

  1. custom(20 min.)
  2. filtrationThe mixture was filtered
  3. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-dba950f6e05e49729c70cf265ecaba79
Quelldatensatz
uspto-grants-1989_02
Patentnummer
US04804677

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