HRID618223
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-(2,4-dimethyl-5-nitrophenyl)acetamide, water (24 mL), concentrated sulfuric acid (12 mL), and ethanol (120 mL) was heated at reflux under an atmosphere of nitrogen for 4 hours. The ethanol was evaporated under reduced pressure and the residue partitioned between ethyl acetate (250 mL) and brine (150 mL). The brine solution was reextracted with ethyl acetate. The combined ethyl acetate extracts were then dried over magnesium sulfate. Evaporation afforded a crude product which was flash chromatographed on silica and eluted with ethyl acetate:hexane (1:4) to afford 4.63 g as a pale yellow solid.
WORKUP
后处理
- temperaturewas heated
- temperatureat reflux under an atmosphere of nitrogen for 4 hours
- customThe ethanol was evaporated under reduced pressure
- customthe residue partitioned between ethyl acetate (250 mL) and brine (150 mL)
- dry with materialThe combined ethyl acetate extracts were then dried over magnesium sulfate
- customEvaporation