HRID1577485
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 sample of 3-[(1-ethylpropyl)amino]-6-methyl-2,4-dinitrobenzyl acetate (23.1 g; 0.068 mol) is added to a mixture of concentrated hydrochloric acid (30 ml), water (40 ml) and methanol (320 ml). The reaction mixture is refluxed for 4 hours, cooled down and concentrated in vacuo. It is then diluted with water, extracted with ether, and the ether layer dried. The ether is removed in vacuo to leave a red oil, which readily solidifies to a yellow-orange solid (19.9 g; 98.5%). A similarly prepared and purified sample has a melting point of 51°-54° C.
WORKUP
后处理
- temperatureThe reaction mixture is refluxed for 4 hours
- temperaturecooled down
- concentrationconcentrated in vacuo
- additionIt is then diluted with water
- extractionextracted with ether
- dry with materialthe ether layer dried
- customThe ether is removed in vacuo
- customto leave a red oil, which
- customA similarly prepared
- custompurified sample