Reacción #45767
ord-aa48d38c1d0b4f32810ca3ec04e0401a
Ecuación de reacción
Lawesson's reagent
4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carboxamide
→
compound
Rendimiento 41.8%
4-Cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carbothioamide
Rendimiento 41.8%
Reactivos
Ninguno
Disolventes
Condiciones de reacción
Temperatura
125°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.
Tratamiento posterior
- 1Temperaturaby heating
- 2TemperaturaAfter cooling to room temperature
- 3Otrothe reaction liquid
- 4Concentraciónwas concentrated
- 5Otrothe resulting residue was purified by silica gel column chromatography (eluent, chloroform:ethyl acetate=20:1→10:1)
Procedimiento
Lawesson's reagent (458 mg, 1.13 mmol) was added to a toluene solution of 4-cyano-7-fluoro-5-methyl-6-phenyl-1,3-benzoxazole-2-carboxamide (I-196) (304 mg, 1.03 mmol), followed by heating under reflux in an oil bath at 125° C. for 10 minutes. After cooling to room temperature, the reaction liquid was concentrated, and the resulting residue was purified by silica gel column chromatography (eluent, chloroform:ethyl acetate=20:1→10:1) to obtain the entitled compound (134 mg, 41.8%) as a yellow solid.