Reacción #62352

Ecuación de reacción

acetic acid (2-chloro-5-cyanothiophen-3-ylmethylene)hydrazide

potassium acetate

→

title compound

Rendimiento 10.1%

1-Acetyl-1H-thieno[2,3-c]pyrazole-5-carbonitrile

Rendimiento 10.1%

Disolventes

diphenyl ether

Condiciones de reacción

Tratamiento posterior

1. 1
   Filtraciónfiltration through Celite
2. 2
   Lavadothe filtrate was washed successively with saturated aqueous ammonium chloride and saturated brine
3. 3
   Secadodried over anhydrous magnesium sulfate
4. 4
   Otrothe solvent was evaporated
5. 5
   OtroThe crude product was purified
6. 6
   Otroseparated by silica gel column chromatography (ethyl acetate:n-hexane=1:10-1:5)

Procedimiento

To a solution of 2.53 g of acetic acid (2-chloro-5-cyanothiophen-3-ylmethylene)hydrazide in 22 mL of diphenyl ether were added copper powder and potassium acetate at room temperature, and stirred at 200° C. for 6 hours. Following filtration through Celite, the filtrate was washed successively with saturated aqueous ammonium chloride and saturated brine, dried over anhydrous magnesium sulfate, and the solvent was evaporated. The crude product was purified and separated by silica gel column chromatography (ethyl acetate:n-hexane=1:10-1:5), to afford 215 mg of the title compound as colorless crystals.

Fuente