HRID1038453
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
To 2-chloro-5-nitro-nicotinic acid (1.0 mmol) in methanol was added a solution of sodium methoxide in methanol (2.4 mmol, freshly prepared from sodium metal in methanol). The solution was refluxed for 2 h and the mixture was allowed to cool and concentrated in vacuo. To the resulting residue was added 10% citric acid solution (20 ml) and the solution extracted with ethyl acetate (20 ml). The organic layer was dried (MgSO4) and concentrated in vacuo. The residue was crystallised from water to give a yellow-white solid (73%).
WORKUP
后处理
- temperatureThe solution was refluxed for 2 h
- temperatureto cool
- concentrationconcentrated in vacuo
- additionTo the resulting residue was added 10% citric acid solution (20 ml)
- extractionthe solution extracted with ethyl acetate (20 ml)
- dry with materialThe organic layer was dried (MgSO4)
- concentrationconcentrated in vacuo
- customThe residue was crystallised from water