Reacción #2383803

Ecuación de reacción

thionyl chloride

N-methylpyrazole

chlorosulfonic acid

N2

→

N-methylpyrazole sulfonyl chloride

Disolventes

Water

Condiciones de reacción

Tratamiento posterior

1. 1
   TemperaturaThe reaction mixture was then cooled to room temperature
2. 2
   Temperaturachilled to 0° C
3. 3
   Temperaturawarmed to 70° C. for two hours
4. 4
   TemperaturaThe reaction was cooled to room temperature
5. 5
   Temperaturachilled in an ice bath
6. 6
   Otroto precipitate a white solid which
7. 7
   Filtraciónwas collected by filtration
8. 8
   LavadoThe desired sulfonyl chloride was washed with cold water and hexane

Procedimiento

The N-methylpyrazole sulfonyl chloride was prepared by adding N-methylpyrazole to chilled (0° C.) chlorosulfonic acid. The reaction mixture was allowed to warm to room temperature and then heated to 100° C. overnight under a stream of N2. The reaction mixture was then cooled to room temperature and chilled to 0° C. To this solution was added thionyl chloride (2.5 eq.) and the reaction was stirred at room temperature for 30 min., then warmed to 70° C. for two hours. The reaction was cooled to room temperature and then chilled in an ice bath. Water and ice were slowly added to the reaction mixture to precipitate a white solid which was collected by filtration. The desired sulfonyl chloride was washed with cold water and hexane.

Fuente