反应详情

A mixture of methyl 1H-1,2,4-triazole-3-carboxylate (1 g) and sodium hydride (0.315 g) in anhydrous THF (30 ml) was heated at reflux for 7 h under nitrogen. The reaction was cooled to RT and methyl iodide (1.12 g) was added. The reaction was heated at reflux overnight. The solvent was evaporated and water (10 ml) was added. This was extracted with DCM, the organic layer collected and evaporated to dryness. The residue was dissolved in methanol:DMSO (6 ml, 1:1) and purified by mass directed preparative HPLC (Method A) to give title compound (0.290 g).

1. temperaturewas heated
2. temperatureat reflux for 7 h under nitrogen
3. temperatureThe reaction was heated
4. temperatureat reflux overnight
5. customThe solvent was evaporated
6. additionwater (10 ml) was added
7. extractionThis was extracted with DCM
8. customthe organic layer collected
9. customevaporated to dryness
10. dissolutionThe residue was dissolved in methanol
11. customDMSO (6 ml, 1:1) and purified by mass