HRID1846275
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
CONDITIONS
反应条件
- 温度
- 80 °C
PROCEDURE
实验过程
To a solution of isatoic anhydride (4.00 g, 24.0 mmol) in N,N-dimethyl formamide (80 mL) under nitrogen atmosphere was added 4-sec-butylaniline (3.66 g, 24.0 mmol). The reaction mixture was heated at 80° C. for 24 hours, then the solvent was removed under reduced pressure and the residue was diluted with ethyl acetate, washed with 1 N aqueous solution of sodium hydroxide, water, and dried over sodium sulfate. The crude oil (7 g) was purified by column chromatography (silica gel 230-400 mesh; 10/0 to 4/1 hexanes/EtOAc as eluent) to give pure 2-amino-N-(4-sec-butylphenyl)-benzamide as a brown solid. Yield: 1.8 g (27.3%).
WORKUP
后处理
- customthe solvent was removed under reduced pressure
- additionthe residue was diluted with ethyl acetate
- washwashed with 1 N aqueous solution of sodium hydroxide, water
- dry with materialdried over sodium sulfate
- customThe crude oil (7 g) was purified by column chromatography (silica gel 230-400 mesh; 10/0 to 4/1 hexanes/EtOAc as eluent)