Reacción #2186225

ord-83a9e1f9c1fd47a69643e42b59cc521f

Condiciones de reacción

Temperatura
100°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Filtraciónthe precipitate filtered off
  2. 2
    Lavadowashed with water
  3. 3
    Otroair-dried
  4. 4
    workup.DISSOLUTIONThe crude product was dissolved in heptanes/ethyl acetate (1:1)
  5. 5
    Filtraciónfiltered
  6. 6
    OtroThe filtrate was evaporated

Procedimiento

A stirred mixture of 1-(2,6-dichloro-4-trifluoromethylpheny)-5-ethoxy-4-trifluoromethylthio-1 H-pyrazole-3-carbonitrile (0.55 g, 1.22 mmol) and concentrated sulfuric acid (0.55 ml) was heated at 100° C. for 3 hours. The cooled mixture was added to ice water and the precipitate filtered off, washed with water and air-dried. The crude product was dissolved in heptanes/ethyl acetate (1:1) and filtered. The filtrate was evaporated to give the title compound (0.42 g, yield 73%) as yellowish crystals, mp 161° C., 1H NMR (CDCl3): 1.32 (t, 3H, CH3), 4.68 (q, 2H, OCH2), 5.54 and 6.69 (bs, 2H, C(O)NH2), and 7.77 (s, 2H, Ar—H).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07569516B2uspto-grants-2009_08