Reacción #43406

ord-a158cf89896e435dbf8220d1c6c239ba

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturathe mixture heated
  2. 2
    Temperaturato reflux for 4 hours
  3. 3
    Concentraciónthen concentrated to ca 400 ml
  4. 4
    FiltraciónFiltration
  5. 5
    Lavadowashing with water
  6. 6
    Secadodrying in vacuo over P2O5 for 18 h

Procedimiento

A solution of 2,6-dichloro-5-fluoro-3-pyridinecarboxylic acid (51.12 g, 243 mmol) in methanol (400 ml) was treated with sodium methoxide in methanol (25% w/v, 100 ml, 535 mmol) and the mixture heated to reflux for 4 hours. The cooled mixture was treated with water (400 ml) and acidified to pH2 with aqueous hydrochloric acid (2M) then concentrated to ca 400 ml. Filtration, washing with water and drying in vacuo over P2O5 for 18 h afforded the product as a white solid (32.65 g, 65%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07732460B2uspto-grants-2010_06