Reacción #45670

ord-b781b3d8c25744e5908d183c004c4eaf

Disolventes

Condiciones de reacción

Temperatura
130°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    TemperaturaAfter cooling
  2. 2
    Filtraciónthe precipitated solid was collected by filtration
  3. 3
    Lavadowashed in diethyl ether

Procedimiento

Under nitrogen atmosphere, a mixture of 2-amino-5-bromo-4-fluoro-3-hydroxy-6-methylbenzonitrile (I-75) (6.67 g, 27.2 mmol) and ethyl triethoxyacetate (24.0 g, 54.4 mmol) was stirred at 130° C. for 15 hours. After cooling, n-hexane was added to the reaction liquid, and the precipitated solid was collected by filtration. The obtained solid was suspended and washed in diethyl ether to obtain the entitled compound (7.10 g, 80%) as a pale dark brown solid.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07737166B2uspto-grants-2010_06