HRID1356663
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
4′-Fluoro-2′-nitro-p-toluenesulfonanilide sodium salt (66.46 g (200 mmol)) was dissolved in DMF (66 ml). To this, under heating in an oil bath kept at 120° C., isopropyl iodide (102.0 g (600 mmol)) was added over a period of 20 minutes. The resulting mixture was left to cool to room temperature, mixed with 1% aqueous sodium hydroxide solution and stirred. The resulting crystals were filtered, washed with water and ethanol, successively. The crude crystals thus obtained were recrystallized from ethyl acetate to give 30.58 g (43%) of the title compound as pale yellow crystals.
WORKUP
后处理
- temperatureTo this, under heating in an oil bath
- customkept at 120° C.
- waitThe resulting mixture was left
- filtrationThe resulting crystals were filtered
- washwashed with water and ethanol
- customThe crude crystals thus obtained
- customwere recrystallized from ethyl acetate