Reacción #2186222
ord-2a77e91c6c32445498e64bc6d139404f
Ecuación de reacción
5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulfonyl-1 H-pyrazole-3-carbonitrile
sulfuric acid
→
title compound
Rendimiento 83.0%
5-Amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulfonyl-1H-pyrazole-3-carboxylic acid amide
Rendimiento 83.0%
Reactantes
Reactivos
Ninguno
Condiciones de reacción
Temperatura
100°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1Filtraciónthe precipitate filtered off
- 2Lavadowashed with water
- 3Otroair-dried
- 4OtroPurification by flash chomatography (silica, chloroform)
Procedimiento
A stirred mixture of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-4-trifluoromethylsulfonyl-1 H-pyrazole-3-carbonitrile (1.06 g, 2.21 mmol) and concentrated sulfuric acid (1 ml) was heated to 100° C. for 3 hours. The cooled mixture was added to ice water and the precipitate filtered off, washed with water and air-dried. Purification by flash chomatography (silica, chloroform) gave the title compound (0.869 g, yield 83%) as off-white crystals, mp 217° C., 1H NMR (DMSO-d6): 7.39 (bs, 2H, NH2), 7.57 and 7.78 (bs, 2H, C(O)NH2), and 8.25 (s, 2H, Ar—H).