反应详情

10 ml of concentrated HCl is added to a solution of 6-(3,5-dichlorophenylthio)-3-nitropicolinonitrile (3.4 g, 0.01 mol) in 50 ml of methanol under stirring. The reaction medium is refluxed, added together with 1.68 g (0.03 mol) of iron and stirred for 10 minutes. After returning to room temperature, the reaction mixture is added together with 100 ml of ethyl acetate and 50 ml of water. The pH is adjusted to 10 using 30% soda solution and the organic phase is extracted and then dried on anhydrous sodium sulfate before being concentrated. The residue is purified by silica gel chromatography (ethyl acetate/petroleum ether) to yield, after concentration of the fractions, 2.82 g (91%) of a yellow solid.

1. temperatureThe reaction medium is refluxed
2. stirringstirred for 10 minutes
3. customAfter returning to room temperature
4. extractionthe organic phase is extracted
5. dry with materialdried on anhydrous sodium sulfate
6. concentrationbefore being concentrated
7. customThe residue is purified by silica gel chromatography (ethyl acetate/petroleum ether)
8. customto yield