HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → 5-Methyl-2-methylsulfanyl-7-phenyl-[1,2,4]triazolo[1,5-a]pyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Benzoylacetone | HCID 7166 | — |
| Reactant | HCID 178503514 | HCID 178503514 | — |
| Solvent | Butyl Chloride | HCID 8005 | — |
| Product | 5-Methyl-2-methylsulfanyl-7-phenyl-[1,2,4]triazolo[1,5-a]pyrimidine | HCID 1255801 | 27.2% |
Reaction Steps
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.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05127936 |
| Source dataset | uspto-grants-1992_07 |
| ORD ID | ord-e376680b4efa41c9b2eae7a05bfd0d1b |
| Source note | uspto-grants-1992_07 |