反应详情

A mixture of 2,4-dihydro-4-methy-5-(4-pyridyl)-3H-1,2,4-triazole-3-thione (4.19 g, 2.18×10-2 mole), K2CO3 (3.01 g, 2.18×10-2 mole), methyl iodide (1.5 ml, 2.4×10-2 mole), and acetone (65 ml) was stirred and warmed to reflux. After refluxing overnight, the solvent was evaporated at reduced pressure and the concentrate was treated with water. The aqueous mixture was extracted with EtOAc three times. The EtOAc extracts were combined, washed with saturated aqueous NaCl, and dried over anhydrous Na2SO4. The drying agent was removed by filtration and the filtrate was evaporated at reduced pressure to yield the desired product.

1. temperaturewarmed to reflux
2. temperatureAfter refluxing overnight
3. customthe solvent was evaporated at reduced pressure
4. additionthe concentrate was treated with water
5. extractionThe aqueous mixture was extracted with EtOAc three times
6. washwashed with saturated aqueous NaCl
7. dry with materialdried over anhydrous Na2SO4
8. customThe drying agent was removed by filtration
9. customthe filtrate was evaporated at reduced pressure