HRID37493
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
In 5 ml of ethanol was dissolved 160 mg of 3,4-diethoxycarbonyl-2-fluoro-5-nitro-6-phenylpyridine, and 120 mg (5 eq.) of reduced iron was added to the solution, followed by addition of 0.5 ml (20 eq.) of acetic acid. After the mixture was refluxed for 30 minutes, the solvent was distilled off. The residue was neutralized with sodium hydrogencarbonate, followed by extraction with ethyl acetate. After the precipitate was removed by filtration, the obtained organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried. Then, the solvent was distilled off.
WORKUP
后处理
- additionwas added to the solution
- temperatureAfter the mixture was refluxed for 30 minutes
- distillationthe solvent was distilled off
- extractionfollowed by extraction with ethyl acetate
- customAfter the precipitate was removed by filtration
- washthe obtained organic layer was washed with water
- dry with materiala saturated aqueous solution of sodium chloride, and dried
- distillationThen, the solvent was distilled off