Reacción #974782

ord-a7e9d0c8acb0496eaffb383fe0370721

Reactivos

Ninguno

Disolventes

Condiciones de reacción

Temperatura
0°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONTo this white suspension was added, over 5 min
  2. 2
    workup.WAITat RT for 2.5 h
  3. 3
    FiltraciónThe white salt was filtered
  4. 4
    Otrodried under vacuum
  5. 5
    workup.DISSOLUTIONThe salt was dissolved into 20 ml H2O
  6. 6
    workup.ADDITIONvery slowly treated with about 200 ml saturated aqueous KHCO3
  7. 7
    OtroA white solid precipitated out of the purple solution
  8. 8
    FiltraciónThe solid was filtered
  9. 9
    Otrodried under vacuum

Procedimiento

9.14 g (97.11 mmol) of 4-methylpyrimidine was slowly added to a 0° C. solution of 8.75 g HCl in 40 ml EtOH. To this white suspension was added, over 5 min, 61 ml of a 10-20% by weight solution of ethyl nitrite in EtOH. The reaction was stirred at 0° C. for 10 min and then at RT for 2.5 h. The white salt was filtered and dried under vacuum. The salt was dissolved into 20 ml H2O and very slowly treated with about 200 ml saturated aqueous KHCO3. A white solid precipitated out of the purple solution. The solid was filtered and dried under vacuum to yield the titled compound.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08247430B2uspto-grants-2012_08