HRID487200
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 2,5-dichloro-3-nitrobenzoic acid (23.6 g, 100 mmol), powdered potassium carbonate (41.1 g, 300 mmol), and 4-(aminoethyl)benzoic acid (60.04 g, 400 mmol) in 250 ml of methanol was refluxed under argon for 18 hours. The reaction mixture was poured into 650 ml of 10% aqueous hydrochloric acid solution. The solid was collected and triturated with ethyl acetate. The ethyl acetate extract was decanted, dried with magnesium sulfate and concentrated in vacuo to give 20.15 g (57.5%) of the title compound; mp 255°-257° C.
WORKUP
后处理
- temperaturewas refluxed under argon for 18 hours
- customThe solid was collected
- customtriturated with ethyl acetate
- extractionThe ethyl acetate extract
- customwas decanted
- dry with materialdried with magnesium sulfate
- concentrationconcentrated in vacuo