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2-(3'-Methoxy-3-nitro-biphenyl-4-yl)-malonic acid dimethyl ester → 3'-Methoxy-3-nitrobiphenyl-4-acetic acid

HRID 1744361
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1744361
C[O:2][C:3](=[O:26])[CH:4]([C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][CH3:22])[CH:16]=2)=[CH:11][C:10]=1[N+:23]([O-:25])=[O:24])C(OC)=O>Cl>[CH3:22][O:21][C:17]1[CH:16]=[C:15]([C:12]2[CH:13]=[CH:14][C:9]([CH2:4][C:3]([OH:26])=[O:2])=[C:10]([N+:23]([O-:25])=[O:24])[CH:11]=2)[CH:20]=[CH:19][CH:18]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 1

HCID 106898032-(3'-Methoxy-3-nitro-biphenyl-4-yl)-malonic acid dimethyl ester

Produkt 1

HCID 107556933'-Methoxy-3-nitrobiphenyl-4-acetic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

2-(3′-Methoxy-3-nitro-biphenyl-4-yl)-malonic acid dimethyl ester (4.4023 gms.) is suspended in 45 mL of 6N HCl and heated at 110° C. for 4 days. The reaction mixture is cooled to room temperature and the precipitate is collected by filtration. As the solid material is in rather large chunks, the solid purification is simplified by first dissolving the solid chunks in an excess of hot methanol, and subsequently concentrating the solution in vacuo to get a more manageable powder. This powder is then triturated with approximately 10 mL of methanol and filtered yielding (3′-methoxy-3-nitro-biphenyl-4-yl)-acetic acid in the amount of 2.0120 gms.

Aufarbeitung

  1. temperatureThe reaction mixture is cooled to room temperature
  2. filtrationthe precipitate is collected by filtration
  3. customthe solid purification
  4. dissolutionby first dissolving the solid chunks in an excess of hot methanol
  5. concentrationsubsequently concentrating the solution in vacuo
  6. customto get a more manageable powder
  7. customThis powder is then triturated with approximately 10 mL of methanol
  8. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-58851336104440e8892ab0b7f0d3bbe9
Quelldatensatz
uspto-grants-2006_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07015220B2

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