تفاعل #65786

معادلة التفاعل

2-chloro-3,4-diethoxycarbonyl-5-nitro-6-(4-nitrophenyl)pyridine

hydrochloric acid

→

title compound

المردود 74.2%

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

المردود 74.2%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe mixture was heated
2. 2
   درجة الحرارةunder reflux for 20 minutes
3. 3
   تركيزAfter the reaction mixture was concentrated
4. 4
   استخلاصextraction with ethyl acetate
5. 5
   غسيلThe extract was washed with an aqueous solution of sodium hydrogencarbonate
6. 6
   تجفيفan aqueous solution of sodium chloride consecutively, and dried over magnesium sulfate
7. 7
   تركيزAfter concentration

الإجراء التجريبي

In 20ml of ethanol were suspended 0.91 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-(4-nitrophenyl)pyridine and 1.11 g of reduced iron, and the suspension was heated to 60° C. After 4.7 ml of conc. hydrochloric acid was added, the mixture was heated under reflux for 20 minutes. After the reaction mixture was concentrated, extraction with ethyl acetate was conducted. The extract was washed with an aqueous solution of sodium hydrogencarbonate and an aqueous solution of sodium chloride consecutively, and dried over magnesium sulfate. After concentration, the residue was subjected to silica gel column chromatography (eluent:chloroform/methanol 40:1), to give 0.58 g of the title compound as yellow prisms.

المصدر