反应 #2383803

反应方程式

thionyl chloride

N-methylpyrazole

chlorosulfonic acid

N2

→

N-methylpyrazole sulfonyl chloride

溶剂

Water

反应条件

后处理

1. 1
   温度The reaction mixture was then cooled to room temperature
2. 2
   温度chilled to 0° C
3. 3
   温度warmed to 70° C. for two hours
4. 4
   温度The reaction was cooled to room temperature
5. 5
   温度chilled in an ice bath
6. 6
   其他to precipitate a white solid which
7. 7
   过滤was collected by filtration
8. 8
   洗涤The desired sulfonyl chloride was washed with cold water and hexane

实验过程

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.

来源