반응 #65786

반응 방정식

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

hydrochloric acid

→

title compound

수율 74.2%

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

수율 74.2%

용매

ethanol

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도under reflux for 20 minutes
3. 3
   농축After the reaction mixture was concentrated
4. 4
   추출extraction with ethyl acetate
5. 5
   세척The extract was washed with an aqueous solution of sodium hydrogencarbonate
6. 6
   건조an aqueous solution of sodium chloride consecutively, and dried over magnesium sulfate
7. 7
   농축After concentration

실험 절차

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.

출처