تفاعل #65762

معادلة التفاعل

hydrochloric acid

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

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

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwas added
2. 2
   درجة الحرارةthe mixture was refluxed
3. 3
   درجة الحرارةAfter heating for 20 minutes
4. 4
   workup.DISTILLATIONthe solvent was distilled off
5. 5
   استخلاصfollowed by extraction with ethyl acetate
6. 6
   ترشيحAfter the precipitate was filtered off
7. 7
   غسيلthe obtained organic layer was washed with water
8. 8
   تجفيفa saturated aqueous solution of sodium chloride, and dried
9. 9
   workup.DISTILLATIONThereafter, the solvent was distilled off

الإجراء التجريبي

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.

المصدر