反应详情

0.55 g (2.5 mmol) of ethyl 3-(4-methoxyphenyl)-3-oxopropanoate, 10 ml of ethanol and 0.3 ml (3 mmol) of piperidine are added respectively to 1 g (2.5 mmol) of tert-butyl 4-(4-(3-amino-2-cyano-3-thioxoprop-1-enyl)-3-nitrophenyl)piperazine-1-carboxylate. The reaction mixture is stirred at room temperature for 5 h and then 0.31 ml (5 mmol) of methyl iodide is added. After 12 h of stirring, 3 ml of acetic acid is added and the reaction medium is carried at 50° C. for 24 hours. After returning to room temperature, the solvents are evaporated and the residue is purified by silica gel chromatography (eluent: 3:7 cyclohexane/ethyl acetate) to yield 1.3 g (83%) of tert-butyl 4-(4-(3-cyano-5-(ethoxycarbonyl)-6-(4-methoxyphenyl)-2-(methylthio)-1,4-dihydropyridine-4-yl)-3-nitrophenyl)piperazine-1-carboxylate in the form of a light yellow powder.

1. stirringAfter 12 h of stirring
2. waitthe reaction medium is carried at 50° C. for 24 hours
3. customAfter returning to room temperature
4. customthe solvents are evaporated
5. customthe residue is purified by silica gel chromatography (eluent: 3:7 cyclohexane/ethyl acetate)