反应详情

Into a 10-mL sealed tube, was placed a solution of 3-methyl-1H-pyrazole-4-carbonitrile (compound 257.3, 2.0 g, 18.7 mmol) in DCE (6 mL). NIS (4.20 g, 18.7 mmol) was added to the reaction and the mixture was irradiated with microwave radiation for 1 h at 150° C. The reaction was cooled, then carefully quenched with aqueous Na2S2O3 (sat., 20 mL). The mixture was partitioned and the aqueous layer was extracted with ethyl acetate (100 mL). The combined organic layers were washed with brine (5×30 mL), dried (Na2SO4), filtered and concentrated under reduced pressure. The residue was purified by silica gel chromatography with ethyl acetate/petroleum ether (1:10) as eluent to obtain the title compound as a yellow solid (900 mg, 21%).

1. customInto a 10-mL sealed tube
2. customthe mixture was irradiated with microwave radiation for 1 h at 150° C
3. temperatureThe reaction was cooled
4. customcarefully quenched with aqueous Na2S2O3 (sat., 20 mL)
5. customThe mixture was partitioned
6. extractionthe aqueous layer was extracted with ethyl acetate (100 mL)
7. washThe combined organic layers were washed with brine (5×30 mL)
8. dry with materialdried (Na2SO4)
9. filtrationfiltered
10. concentrationconcentrated under reduced pressure
11. customThe residue was purified by silica gel chromatography with ethyl acetate/petroleum ether (1:10) as eluent