反应详情

温度

100 °C

0.1 g (0.40 mmol) of methyl 2-cyano-3-(methylsulfanyl)-3-(3-pyridinylamino)-2-propenoate and 0.065 g (0.40 mmol) of 2-cyclopentylethanamidine hydrochloride and 0.16 g (1.60 mmol) of triethylamine are dissolved in 0.5 ml of DMF and stirred at 100° C. overnight. After cooling, the mixture is diluted with 10 ml of water and extracted with dichloromethane. The organic phase is dried over sodium sulfate and concentrated in vacuo, and the residue is purified by flash chromatography (mobile phase: dichloromethane/methanol 200:1, 100:1, 50:1). 78 mg (64% of theory) of the product are obtained as a colorless solid.

1. temperatureAfter cooling
2. extractionextracted with dichloromethane
3. dry with materialThe organic phase is dried over sodium sulfate
4. concentrationconcentrated in vacuo
5. customthe residue is purified by flash chromatography (mobile phase: dichloromethane/methanol 200:1, 100:1, 50:1)
6. custom78 mg (64% of theory) of the product are obtained as a colorless solid