반응 #65773

반응 방정식

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

hydrochloric acid

→

title compound

수율 91.3%

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

수율 91.3%

용매

ethanol

반응 조건

후처리

1. 1
   온도the mixture was heated for 30 minutes
2. 2
   온도under reflux
3. 3
   농축After the reaction mixture was concentrated
4. 4
   추출the residue was extracted with ethyl acetate
5. 5
   세척by washing with an aqueous solution of sodium hydrogencarbonate
6. 6
   건조an aqueous solution of sodium chloride and drying over magnesium sulfate
7. 7
   농축After the extract was concentrated under reduced pressure

실험 절차

In 8 ml of ethanol were suspended 0.37 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-(3-nitrophenyl)pyridine and 0.45 g of reduced iron, and the suspension was heated to 60° C. After 1.9 ml of conc. hydrochloric acid was added thereto, the mixture was heated for 30 minutes under reflux. After the reaction mixture was concentrated, the residue was extracted with ethyl acetate, followed by washing with an aqueous solution of sodium hydrogencarbonate and an aqueous solution of sodium chloride and drying over magnesium sulfate. After the extract was concentrated under reduced pressure, the residue was subjected to silica gel column chromatography (eluent: chloroform/methanol 40:1) to give 0.29 g of the title compound as a yellowish orange viscous oily substance.

출처