HRID1704268
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 mixture of 1-chloro-2,6-dinitrobenzene (30 grams), anhydrous potassium fluoride (35 grams), and dimethylformamide (50 ml.) is refluxed for twenty-four hours. The reaction mixture is poured into water (250 ml.) and extracted with ether (3 × 100 ml.). The combined ether extracts are dried with anhydrous sodium sulfate. Removal of the solvent leaves brown solid. Chromatography of the solid on silica gel with methylene chloride as the elutant gives a light yellow solid after recrystallization from pentane-methylene chloride. (20.30 grams, melting point 59°). Mass spectrum (70 ev) mol. ion 186 m/e.
WORKUP
后处理
- temperatureis refluxed for twenty-four hours
- extractionextracted with ether (3 × 100 ml.)
- dry with materialThe combined ether extracts are dried with anhydrous sodium sulfate
- customRemoval of the solvent
- customleaves brown solid
- customafter recrystallization from pentane-methylene chloride