Oxalic Acid → HCID 15524196, Verbindung

HRID 1530844Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1530844
[Br:1][C:2]1[CH:11]=[C:10]([N+:12]([O-])=O)[C:9]([NH2:15])=[C:8]2[C:3]=1[CH2:4][CH2:5][N:6]([CH2:16][CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH2:7]2.[C:25](O)(=[O:29])[C:26](O)=[O:27]>Cl>[Br:1][C:2]1[C:3]2[CH2:4][CH2:5][N:6]([CH2:16][CH2:17][CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)[CH2:7][C:8]=2[C:9]2[NH:15][C:25](=[O:29])[C:26](=[O:27])[NH:12][C:10]=2[CH:11]=1

Komponenten

4

Edukt 2

HCID 971Oxalic AcidHCID 155241945-Bromo-1,2,3,4-tetrahydro-7-nitro-2-(3-phenylpropyl)-8-isoquinolinamine

Produkt 1

HCID 15524196HCID 15524196, VerbindungAusbeute 60,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

A solution of the product from Example 12 (0.98 g, 2.72 mmol) in 3N HCl (35 mL) was treated with oxalic acid (0.36 g, 2.86 mmol) and refluxed for five hours. When cool to room temperatures the precipitate was filtered, suspended in water (70 mL) and basifyed to pH 8. The solids were filtered, and dried to give the title compound (0.68 g, 60%) as a brown solid, mp=288-293° C.

Aufarbeitung

  1. temperaturerefluxed for five hours
  2. temperatureWhen cool to room temperatures the precipitate
  3. filtrationwas filtered
  4. filtrationThe solids were filtered
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-38109f6d34a34d44adad87768b9167f6
Quelldatensatz
uspto-grants-2001_03
Patentnummer
US06197771B1

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