Reacción #502101

ord-548706e46c1f4ed79f3d42a458df1076

Condiciones de reacción

Temperatura
105°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturacooled to ambient temperature
  2. 2
    Concentraciónconcentrated under reduced pressure
  3. 3
    Otrois taken up between dichloromethane and water at 0° C.
  4. 4
    workup.ADDITIONa 30% aqueous solution of NH4OH is added until a basic pH
  5. 5
    Otrois obtained
  6. 6
    OtroThe organic phase is separated
  7. 7
    Secadodried over magnesium sulphate
  8. 8
    Concentraciónconcentrated under reduced pressure

Procedimiento

8.78 g of ethyl[2-imino-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1H-pyridin-1-yl]acetate hydrobromide in 20 ml of POCl3 are placed in a round-bottomed flask. The reaction mixture is heated at 105° C. for 16 h, cooled to ambient temperature and concentrated under reduced pressure. The residue is taken up between dichloromethane and water at 0° C., and a 30% aqueous solution of NH4OH is added until a basic pH is obtained. The organic phase is separated, dried over magnesium sulphate and concentrated under reduced pressure. 4.3 g of compound are obtained.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08088765B2uspto-grants-2012_01