反応 #65762

反応方程式

hydrochloric acid

2-chloro-3,4-diethyoxycarbonyl-6-(4-methoxyphenyl)-5nitropyridine

→

3-Amino-6-chloro-4,5-diethoxycarbonyl-2-(4-methoxyphenyl)pyridine

溶媒

ethanol

反応条件

後処理

1. 1
   workup.ADDITIONwas added
2. 2
   温度the mixture was refluxed
3. 3
   温度After heating for 20 minutes
4. 4
   workup.DISTILLATIONthe solvent was distilled off
5. 5
   抽出followed by extraction with ethyl acetate
6. 6
   ろ過After the precipitate was filtered off
7. 7
   洗浄the obtained organic layer was washed with water
8. 8
   乾燥a saturated aqueous solution of sodium chloride, and dried
9. 9
   workup.DISTILLATIONThereafter, the solvent was distilled off

実験手順

In 4 ml of ethanol was dissolved 280 mg of 2-chloro-3,4-diethyoxycarbonyl-6-(4-methoxyphenyl)-5nitropyridine, whereto 340 mg(8.9 eq.) of reduced iron was added. After the mixture was heated to 60° C., 1.5 ml of conc. hydrochloric acid was added dropwise and the mixture was refluxed. After heating for 20 minutes, the solvent was distilled off. The residue was neutralized with an aqueous solution of sodium hydrogencarbonate, followed by extraction with ethyl acetate. After the precipitate was filtered off, the obtained organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried. Thereafter, the solvent was distilled off.

出典