Reaktion #56033

ord-22bae4bf65454d5684f0495640d96b1c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux temperature
  2. 2
    workup.ADDITIONAfter the addition
  3. 3
    Temperaturthe mixture is refluxed for an additional hour
  4. 4
    workup.ADDITIONpoured onto ice
  5. 5
    Sonstige2-butylamino-5-cyano-6-methyl-3-pyridine-carboxylic acid, ethyl ester precipitates

Vorschrift

112 g of 2-chloro-5-cyano-6-methyl-3-pyridine-carboxylic acid, ethyl ester (0.5 mol) are dissolved in 300 ml of alcohol and 73 g of n-butylamine are dropped in at reflux temperature with stirring. After the addition is completed, the mixture is refluxed for an additional hour and then poured onto ice. 2-butylamino-5-cyano-6-methyl-3-pyridine-carboxylic acid, ethyl ester precipitates. Yield 116 g (89%); m.p. 61°-63° C. (petrol ether).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04223142uspto-grants-1980_09