反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of N-ethyl-4-amino-3-(2,4-difluorophenylthio)benzamide (0.84 g) and methanesulfonyl chloride (0.57 g) in pyridine (5 ml) was stirred at room temperature overnight. The reaction mixture was concentrated. The residue was dissolved in ethyl acetate, washed with dilute hydrochloric acid, dried and evaporated. The residue obtained was dissolved in methanol and treated with potassium hydroxide (0.4 g). The solution was concentrated and the residue was dissolved in water. The aqueous solution was acidified with dilute hydrochloric acid and extracted with chloroform. The extract was washed with water, dried, and evaporated. The residual solid was recrystallized from ethanol to give N-ethyl-3-(2,4-difluorophenylthio)-4-(methanesulfonamido)benzamide (0.67 g).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated
- dissolutionThe residue was dissolved in ethyl acetate
- washwashed with dilute hydrochloric acid
- customdried
- customevaporated
- customThe residue obtained
- concentrationThe solution was concentrated
- dissolutionthe residue was dissolved in water
- extractionextracted with chloroform
- washThe extract was washed with water
- customdried
- customevaporated
- customThe residual solid was recrystallized from ethanol