Reacción #73180

ord-ea79b23d79d04a57bcd85d8bc5c31064

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturawith cooling, in the course of which the product
  2. 2
    Otroprecipitates out
  3. 3
    FiltraciónIt is filtered off
  4. 4
    Lavadowashed with 300 ml of water
  5. 5
    Otrosubsequently dried at 35-40° C.

Procedimiento

165.5 g (0.98 mol) of 2-hydroxymethyl-3-pyridinecarboxamide are heated together with 270 ml of phosphorus oxychloride to 90-100° C. for 1 hour. The reaction mixture is cooled to room temperature and subsequently added dropwise to approx. 800 ml of water at 50-60° C. After the phosphorus oxychloride has been hydrolyzed, the mixture is neutralized with sodium hydroxide solution with cooling, in the course of which the product precipitates out. It is filtered off, washed with 300 ml of water and subsequently dried at 35-40° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08541450B2uspto-grants-2013_09