反应详情

温度

20 °C

4.3 g of guanidinium chloride are added to a suspension of 5.2 g of potassium tert-butoxide in 100 cm3 of dimethylformamide. The reaction mixture is stirred under an inert atmosphere at a temperature in the region of 20° C. for 1 hour, followed by addition of a solution of 2 g of ethyl (2-methyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetate in 20 cm3 of dimethylformamide. The reaction mixture is stirred at a temperature in the region of 20° C. for 16 hours, followed by addition of 100 cm3 of water. The pH is adjusted to 8 by adding 50 cm3 of 1N hydrochloric acid, and the mixture is concentrated under reduced pressure (0.6 kPa) at a temperature in the region of 30° C. The evaporation residue is taken up in water and then filtered. 0.35 g of N-[(2-methyl-3-oxo-2,3-dihydro-1H-isoindol-1-yl)acetyl]guanidine is thus obtained in the form of an off-white solid melting at 214° C. Mass spectrum EI: m/e 246 (M+), m/e 159 (base peak), m/e 146.

1. stirringThe reaction mixture is stirred at a temperature in the region of 20° C. for 16 hours
2. concentrationthe mixture is concentrated under reduced pressure (0.6 kPa) at a temperature in the region of 30° C
3. filtrationfiltered