反应详情

A mixture of 7.0 g (71 mmol) 3,5-diamino-1,2,4-triazole and 12.0 g (74 mmol) benzoylacetone in 100 ml of glacial acetic acid was heated at reflux 2 hours. After cooling, methylene chloride (200 ml) was added followed by the addition of excess water. The organic layer was separated, washed with water, brine, dried over magensium sulfate and evaporated in vacuo to give a solid residue to which ethyl acetate was added. Filtering gave 16.0 g of crude 5-methyl-7-phenyl-1,2,4-triazolo[1,5-a]pyrimidin-2-amine (m.p. 246°-250° C.) which was used directly in the next step.

1. temperaturewas heated
2. temperatureat reflux 2 hours
3. temperatureAfter cooling
4. customThe organic layer was separated
5. washwashed with water, brine
6. dry with materialdried over magensium sulfate
7. customevaporated in vacuo
8. customto give a solid residue to which ethyl acetate
9. additionwas added
10. filtrationFiltering