反应详情

A 5.38 g portion of N-(5-propyl-1H-pyrazol-3-yl)acetamidoxime was dissolved in 45 ml of N,N-dimethylacetamide. With cooling on an ice bath, to this were added 2.39 ml of pyridine and 5.63 g of p-toluenesulfonic acid chloride, followed by 30 minutes of stirring at the same temperature and additional 3 hours of stirring at room temperature. The resulting reaction mixture was added to 350 ml of water and extracted with chloroform. After distilling off chloroform from the organic layer under a reduced pressure, the thus obtained residue was dissolved in 135 ml of methanol, mixed with 2.39 ml of pyridine and then heated under reflux for 2 hours.

1. temperatureWith cooling on an ice bath
2. stirringof stirring at room temperature
3. customThe resulting reaction mixture
4. extractionextracted with chloroform
5. distillationAfter distilling off chloroform from the organic layer under a reduced pressure
6. dissolutionthe thus obtained residue was dissolved in 135 ml of methanol
7. additionmixed with 2.39 ml of pyridine
8. temperatureheated
9. temperatureunder reflux for 2 hours