Reaktion #575723

ord-67b3606ed97745088224a32eb7d53c20

Reaktionsgleichung

O=C(O)c1ccc(CCl)cc1
α-chloroparatoluic acid
CCNCC
diethylamine
CCN(CC)Cc1ccc(C(=O)O)cc1
α-diethylamino-paratoluic Acid
Ausbeute 63.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto reflux for 48 hours
  2. 2
    SonstigeThe solvent is evaporated off under vacuum
  3. 3
    Sonstigethe residue is purified by chromatography on silica gel column (CH2Cl2/MeOH 60/40
  4. 4
    SonstigeThe product is obtained in the form of a white powder
  5. 5
    Sonstigeafter precipitation from hexane

Vorschrift

1 g (1 equivalent) of α-chloroparatoluic acid and 1.22 mL (2 equivalents) of diethylamine are placed in solution in 30 mL of acetonitrile. The reaction mixture is taken to reflux for 48 hours. The solvent is evaporated off under vacuum and the residue is purified by chromatography on silica gel column (CH2Cl2/MeOH 60/40 then pure MeOH). The product is obtained in the form of a white powder after precipitation from hexane. (Yield=63%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06972343B1uspto-grants-2005_12