HRID2290184
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
To a stirred suspension of 65.11 g (0.195 mol) of 5-bromo-6-methylsulfamoyl-N-acetylindoline in 200 ml dioxane was added 146 ml (1.75 mol) concentrated hydrochloric acid. The mixture was stirred and refluxed for 1.5 hours and allowed to cool. The mixture was then concentrated under reduced pressure, cooled in an ice bath and neutralized with 10% sodium hydroxide solution to pH 7. The resulting white precipitate was filtered, washed several times with water and allowed to dry overnight to give 55.92 g (98% by weight yield) of 5-bromo-6-methylsulfamoylindoline.
WORKUP
后处理
- temperaturerefluxed for 1.5 hours
- temperatureto cool
- concentrationThe mixture was then concentrated under reduced pressure
- temperaturecooled in an ice bath
- filtrationThe resulting white precipitate was filtered
- washwashed several times with water
- customto dry overnight