反应详情

A suspension of 14.7 g of 3-amino-5-methyl-s-triazole and 26.8 g of ethyl acetylenedicarboxylate in 120 ml of ethanol was refluxed for three hours, the reaction mixture was allowed to stand at room temperature for one hour, and the formed crystals were collected by filtration. The filtrate was concentrated and the residue was recrystallized from dichloromethane, and the crystals were joined with those obtained above. Purification by silica gel chromatography gave 10.8 g of the objective compound as colorless crystals.

1. temperaturewas refluxed for three hours
2. filtrationthe formed crystals were collected by filtration
3. concentrationThe filtrate was concentrated
4. customthe residue was recrystallized from dichloromethane
5. customthose obtained above
6. customPurification by silica gel chromatography