反応 #65786

反応方程式

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

hydrochloric acid

→

title compound

収率 74.2%

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

収率 74.2%

溶媒

ethanol

反応条件

後処理

1. 1
   温度the mixture was heated
2. 2
   温度under reflux for 20 minutes
3. 3
   濃縮After the reaction mixture was concentrated
4. 4
   抽出extraction with ethyl acetate
5. 5
   洗浄The extract was washed with an aqueous solution of sodium hydrogencarbonate
6. 6
   乾燥an aqueous solution of sodium chloride consecutively, and dried over magnesium sulfate
7. 7
   濃縮After concentration

実験手順

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.

出典