反应详情

To 50 ml of stirring glacial acetic acid, 2.5 g (19.2 mmol) of 3-amino-5-methylthio-1,2,4-triazole and 3.1 g (19.1 mmol) of benzoylacetone was added followed by heating at reflux for 2 h. The solvent was evaporated in vacuo and excess water added to the residue followed by extraction with 200 ml of ethyl acetate. The extract was washed with water, saturated sodium bicarbonate, brine, dried over magnesium sulfate and evaporated in vacuo to give an oil. Addition of n-butyl chloride resulted in crystallization of a solid which was filtered and washed with n-butyl chloride to give 1.33 g of the pure title compound, m.p. 121°-123° C.

1. temperatureby heating
2. temperatureat reflux for 2 h
3. customThe solvent was evaporated in vacuo and excess water
4. additionadded to the residue
5. extractionfollowed by extraction with 200 ml of ethyl acetate
6. washThe extract was washed with water, saturated sodium bicarbonate, brine
7. dry with materialdried over magnesium sulfate
8. customevaporated in vacuo
9. customto give an oil
10. customresulted in crystallization of a solid which
11. filtrationwas filtered
12. washwashed with n-butyl chloride