HRID1494840
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
2.54 g of 2-benzyl-4-nitroisoindoline was dissolved in 10 ml of chloroform, and 1.27 g of sodium carbonate was added to the solution. To the mixture was added dropwise 1.30 g of ethyl chloroformate under ice-cooling while stirring. After the addition, the stirring was continued for 20 hours at room temperature. The insoluble materials were removed by filtration and the filtrate was washed with water, 5% hydrochloric acid, and then with water. The mixture was concentrated and recrystallized from a chloroform-ether mixed solvent to obtain 1.73 g of 2-ethoxycarbonyl-4-nitroisoindoline.
WORKUP
后处理
- temperaturecooling
- additionAfter the addition
- customThe insoluble materials were removed by filtration
- washthe filtrate was washed with water, 5% hydrochloric acid
- concentrationThe mixture was concentrated
- customrecrystallized from a chloroform-ether mixed solvent