HRID1287695
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 22.7 g (0.1 mol) of 3'-hydroxy-2-methylbenzanilide, 11.9 g (0.1 mol) of propargylbromide, 10.6 g (0.1 mol) of sodium carbonate and 250 ml of acetone was prepared and the nixture was refluxed for 4 hours with stirring. After cooling, the reaction mixture was filtered and the acetone was removed by distillation. The residual material was dissolved in benzene, washed with water and dehydrated over anhydrous sodium sulfate. The benzene was removed and the product was recrystallized from aqueous ethanol to obtain a 23.2 g (87.7%) of fine white needles having a melting point of 93°-95° C. EXAMPLE 8
WORKUP
后处理
- customwas prepared
- temperaturethe nixture was refluxed for 4 hours
- temperatureAfter cooling
- filtrationthe reaction mixture was filtered
- customthe acetone was removed by distillation
- dissolutionThe residual material was dissolved in benzene
- washwashed with water
- customThe benzene was removed
- customthe product was recrystallized from aqueous ethanol