Ethanol → 4-Aminobenzene-1,3-dioic acid

HRID 1247177

Reaktionsgleichung

Reaktionsgleichung von HRID 1247177
CCO.[N+:4]([C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][C:8]=1[C:16]([OH:18])=[O:17])([O-])=O>[Pd].CC(O)=O>[NH2:4][C:7]1[CH:15]=[CH:14][C:10]([C:11]([OH:13])=[O:12])=[CH:9][C:8]=1[C:16]([OH:18])=[O:17]

Komponenten

5

Edukt 2

HCID 702EthanolHCID 30624384-Nitroisophthalic acid

Produkt 1

HCID 113558524-Aminobenzene-1,3-dioic acidAusbeute 75,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

Into 20 mL EtOH and 20 mL HOAc was dissolved 2 g (9.48 mmol) 4-nitroisophthalic acid, and the solution was subjected to hydrogenation at atmospheric conditions over 1 g of 5% Pd on carbon. After 16 h, mixture was filtered, and filtrate was evaporated. The residue crystallized from methylene chloride-hexane, giving 1.29 g (75%) crystalline desired intermediate.

Aufarbeitung

  1. filtrationmixture was filtered
  2. customfiltrate was evaporated
  3. customThe residue crystallized from methylene chloride-hexane

Quellen und Nachweise

ORD-Eintrag
ord-f1b9c8ee575c45eea6a0a0c2e1b6e831
Quelldatensatz
uspto-grants-2006_10
Patentnummer
US07129245B2

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