HRID1580771
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
7.65 gm (0.05 mol) of 1,4-diamino-2-nitrobenzene were added to 80 ml of absolute tetrahydrofuran and 5.1 gm (0.05 mol) of triethylamine at room temperature to form a solution. While this mixture was being stirred, 7.5 gm (0.05 mol) of malonic acid monoethylester chloride were added dropwise thereto. After termination of the addition, the mixture was stirred at room temperature for another 6 hours. Then the solvent was evaporated in vacuo for the most part. The residue was suctioned off and recrystallized once from ethanol/activated charcoal and a second time from water. The product had a melting point of 133°-136°C.
WORKUP
后处理
- customto form a solution
- additionAfter termination of the addition
- stirringthe mixture was stirred at room temperature for another 6 hours
- customThen the solvent was evaporated in vacuo for the most part
- customrecrystallized once from ethanol/activated charcoal