Reacción #164249

ord-92bb9cd27d924c84a9817c351b1d9db8

Disolventes

Condiciones de reacción

Temperatura
170°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroMethod 2—Step a Into a one necked round bottomed flask equipped with a magnetic stirrer
  2. 2
    workup.WAITleft
  3. 3
    Otroto come rt

Procedimiento

Method 2—Step a Into a one necked round bottomed flask equipped with a magnetic stirrer, 5-bromo-2-chlorobenzoic acid (70.0 g, 297.3 mmol), o-phenylenediamine (64.3 g, 594.6 mmol) and methansulfonic acid (140 mL) were placed and heated to 170° C. in order to melt the solids. The system was stirred 5 h at this temperature, then left to come rt. The blue solid was treated with NaOH 35% (200 mL) obtaining a violet suspension (pH 5) that was filtered and washed with NaOH 0.5 M (2 L) and H2O (2 L). The product was dried under vacuum (60° C.), to give 61.6 g of a pure violet solid. (67%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08835648B2uspto-grants-2014_09