反应详情

温度

0 °C

1.5 g (11.3 mmol) 3-amino-5-tert-butylpyrazole dissolved in acetonitrile, was added drop-wise and slowly to a solution of 2.0 g (11.3 mmol) thiocarbonyldiimidazole in 25 ml acetonitrile, at 0° C. The batch was stirred for 20 minutes at 0° C., ammonium acetate (1.6 g, 21.5 mmol) was then added, and the mixture was heated in the microwave for 30 minutes at 90° C. (radiation power 200 Watt/without cooling). The solid formed was suction-isolated, the solution was concentrated and the oily residue (4.3 g) was crudely purified on silica gel (0.9 g yellowish solid)

1. additionwas added drop-wise
2. customat 0° C
3. temperaturethe mixture was heated in the microwave for 30 minutes at 90° C.
4. temperature(radiation power 200 Watt/without cooling)
5. customThe solid formed
6. customwas suction-isolated
7. concentrationthe solution was concentrated
8. customthe oily residue (4.3 g) was crudely purified on silica gel (0.9 g yellowish solid)