Reacción #90258

ord-b16dc701397b4aeaadbfc669e9d5dbcd

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturaat reflux for three hours
  2. 2
    Temperaturaat reflux overnight
  3. 3
    Temperaturato cool to room temperature
  4. 4
    Filtraciónthe copious precipitate was filtered off
  5. 5
    Lavadowashed with water
  6. 6
    Otrodried

Procedimiento

A mixture of 3,4-dimethoxy-5-nitrobenzoic acid (0.53 g, 2.34 mmol) and 1,1-carbonyldiimidazole (0.42 g, 2.59 mmol) was heated in tetrahydrofuran (10 mL) at reflux for three hours and then cooled to room temperature. 2-Trifluoromethyl-nicotinic acid hydrazide (0.53 g, 2.57 mmol) was added in one portion and the yellowish mixture was stirred at reflux overnight and then allowed to cool to room temperature. The mixture was poured onto cold water (100 mL) and the copious precipitate was filtered off, washed with water and dried to give 2-trifluoromethyl-nicotinic acid N′-(3,4-dimethoxy-5-nitro-benzoyl)-hydrazide (0.71 g, 73%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US09446012B2uspto-grants-2016_09