反应详情

A mixture of 13.72 g of 2,3-diamino-4,6-dimethyl-pyridine and 25 g of glycolic acid in 200 ml of toluene was heated under reflux for 3.5 hours, whilst distilling off azeotropically the water formed in the course of the reaction. At the end of this time, the reaction mixture was freed from the toluene by decantation and the oily residue was purified by column chromatography through silica gel, using a gradient elution method, with mixtures of ethanol and ethyl acetate in ratios ranging from 2:3 to 1:1 by volume as a eluent, to give 2.7 g of the title compound, melting at 244°-246° C.

1. temperaturewas heated
2. temperatureunder reflux for 3.5 hours
3. distillationwhilst distilling off azeotropically the water
4. customformed in the course of the reaction
5. customthe oily residue was purified by column chromatography through silica gel
6. washa gradient elution method