Ethanol → Ethyl 4,5-diamino-2-ethoxy-benzoate

HRID 578057Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 578057
C([NH:8][C:9]1[C:19]([N+:20]([O-])=O)=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:11]([O:23][CH2:24][CH3:25])[CH:10]=1)C1C=CC=CC=1.C(O)C>[Pd].C1COCC1>[NH2:8][C:9]1[C:19]([NH2:20])=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:11]([O:23][CH2:24][CH3:25])[CH:10]=1

Komponenten

5

Edukt 2

HCID 702EthanolHCID 67233615Ethyl 4-benzylamino-2-ethoxy-5-nitro-benzoate

Produkt 1

HCID 67229822Ethyl 4,5-diamino-2-ethoxy-benzoate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23938PalladiumKatalysatorHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Palladium on charcoal (3.50 g 10%) was added to the product obtained at (655c) (16.7 g, 46.1 mmol) in 200 mL THF with 200 mL ethanol and the mixture was hydrogenated using a Parr apparatur at 60 psi H2 pressure and 50° C. for 3 h. The mixture was filtered, washed with ethanol and the filtrate concentrated i. vac. The residue was triturated with dichloromethane and evaporated to dryness. The product was reacted without further purification.

Aufarbeitung

  1. customat 60 psi H2 pressure and 50° C.
  2. customfor 3 h
  3. filtrationThe mixture was filtered
  4. washwashed with ethanol
  5. concentrationthe filtrate concentrated i
  6. customThe residue was triturated with dichloromethane
  7. customevaporated to dryness
  8. customThe product was reacted without further purification

Quellen und Nachweise

ORD-Eintrag
ord-f2236cc87619431e88883eb50219acde
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09040565B2

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