HRID1514924
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
- 60 °C
PROCEDURE
实验过程
To a solution of the crude 4-amino-3-iodo-benzoic acid methyl ester in 20 mL of acetic acid was added acetic anhydride (1.25 mL). The reaction was heated at 60° C. for 1 h. The reaction mixture was quenched with water, extracted with ethyl acetate, dried over Na2SO4, and concentrated in vacuo. Purification by flash chromatography (SiO2, 1:3 EtOAc/Hexane) afforded 4-acetylamino-3-iodo-benzoic acid methyl ester: MS (m/z) 320.0 (M+1).
WORKUP
后处理
- customThe reaction mixture was quenched with water
- extractionextracted with ethyl acetate
- dry with materialdried over Na2SO4
- concentrationconcentrated in vacuo
- customPurification by flash chromatography (SiO2, 1:3 EtOAc/Hexane)