反应详情

温度

-20 °C

1.39 g (14.8 mmol) of 3-aminopyridine are dissolved in 50 ml of THF, cooled to −20° C., and 7.4 ml of a 2M solution of n-butyllithium in hexane are added. After stirring for 15 min, 2.00 g (9.84 mmol) of methyl 3,3-bis(methylthio)-2-cyanoacrylate are added. The mixture is warmed to room temperature while stirring and then hydrolyzed with ice-water. The product is extracted with dichloromethane. After drying over sodium sulfate, the solvent is removed in vacuo and the residue is purified by preparative HPLC. 0.44 g (18.1% of theory) of the desired product is obtained.

1. temperatureThe mixture is warmed to room temperature
2. stirringwhile stirring
3. extractionThe product is extracted with dichloromethane
4. dry with materialAfter drying over sodium sulfate
5. customthe solvent is removed in vacuo
6. customthe residue is purified by preparative HPLC