反应详情

温度

50 °C

A suspension of N-(3-methyl-1H-pyrazol-5-yl)acetamide (29.6 g, 0.213 mol), iodic acid (9.3 g, 0.053 mol) and iodine (32.5 g, 0.128 mol) in ethanol (300 mL) was heated at 50° C. for 3 h and cooled to room temperature. The reaction mixture was concentrated in vacuo and taken up in ethyl acetate. The solution was washed twice with 2 M Na2S2O3 followed by brine solution. The organic layer was dried (magnesium sulphate), filtered and concentrated in vacuo. The residue was triturated from diethyl ether, filtered and dried to provide the title compound as a white solid (32.5 g).

1. temperaturecooled to room temperature
2. concentrationThe reaction mixture was concentrated in vacuo
3. washThe solution was washed twice with 2 M Na2S2O3
4. dry with materialThe organic layer was dried (magnesium sulphate)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was triturated from diethyl ether
8. filtrationfiltered
9. customdried