Reacción #8516

ord-9a91687510384f2a99c8906dc00af77d

Disolventes

Condiciones de reacción

Temperatura
70°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe cooled mixture was evaporated
  2. 2
    Extracciónthe residue extracted with cyclohexane
  3. 3
    Otroevaporated

Procedimiento

Phosphoryl chloride (500 microlitres, 1.7 equivalents) was added in one portion to a stirred solution of N′-(2,6-dichloro-4-trifluoromethylphenyl)-chloroacetohydrazide (1.0 g, 3.11 mmol) in toluene (20 ml) and heated at 70° C. under an argon atmosphere for 20 hours. The cooled mixture was evaporated and the residue extracted with cyclohexane. The extracts were combined and evaporated to give the title compound (0.971 g) as an orange oil, NMR 4.4 (s, 2H), 7.55 (s, 2H), 7.7 (s, 1H). The yield was 90%.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07087786B2uspto-grants-2006_08