反応 #46113

反応方程式

4,5-dichloro-2-fluorobenzenesulphonamide

cyclopropylamine

→

title product

4,5-dichloro-2-cyclopropylaminobenzenesulphonamide

溶媒

dioxane

反応条件

後処理

1. 1
   その他The solvent and the excess of amine are removed by distillation under reduced pressure
2. 2
   workup.DISSOLUTIONthe residue is dissolved in methanol (20 mL)
3. 3
   温度The methanolic solution is cooled on an ice bath
4. 4
   workup.ADDITIONwater (60 mL) is added

実験手順

A solution of 4,5-dichloro-2-fluorobenzenesulphonamide (3 g) in dioxane (30 mL) to which cyclopropylamine (3 mL) has been added is heated at 100-110° C. in a hermetically closed vessel for 24 hours. The solvent and the excess of amine are removed by distillation under reduced pressure and the residue is dissolved in methanol (20 mL). The methanolic solution is cooled on an ice bath, and water (60 mL) is added. The precipitate obtained (the title product) is collected by filtration, washed with water and dried. It is used in the following Step without being otherwise purified.

出典