HRID324514
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
Concentrated hydrochloric acid (140μL) was added to a solution of the nitrobenzamide, V.3 (147 mg, 0.30 mmol) in methanol (2 ml). Iron (72 mg) was added and the reaction mixture was heated to 80° C. for 2 hours, before cooling. The reaction mixture was basified (saturated sodium carbonate solution), extracted into ethyl acetate, dried over magnesium sulphate and the solvent removed in vacuo to yield an off-white solid which was purified using flash chromatography(ethyl acetate) to yield the desired 2-aminobenzamide, VI.3 (47 mg, 34%).
WORKUP
后处理
- temperaturebefore cooling
- extractionextracted into ethyl acetate
- dry with materialdried over magnesium sulphate
- customthe solvent removed in vacuo
- customto yield an off-white solid which
- customwas purified