反应详情

Amyl nitrite (13.00 g, 111.0 mmol) was added to a suspension of 5-amino-1-isopropyl-1H-pyrazole-4-carbonitrile (1.77 g, 11.8 mmol) in Diiodomethane (56.0 mL, 695 mmol) at −10° C. in 30 min. The mixture was stirred for 30 min at room temperature and then heated at 100° C. for 2 hours. The mixture was then cooled and concentrated in high vacuum to give a residue which was partitioned between ethyl acetate and 5% Na2S2O5. The organic layer was washed with water, 0.1% of aq HCl, water, brine, dried and concentrated in vacuum. The residue was purified on silica column eluting with 20-30% ethyl acetate in heptane. Yield 1.68 g (55%). MS (ESI+): 262.2

1. temperatureheated at 100° C. for 2 hours
2. temperatureThe mixture was then cooled
3. concentrationconcentrated in high vacuum
4. customto give a residue which
5. customwas partitioned between ethyl acetate and 5% Na2S2O5
6. washThe organic layer was washed with water, 0.1% of aq HCl, water, brine
7. customdried
8. concentrationconcentrated in vacuum
9. customThe residue was purified on silica column
10. washeluting with 20-30% ethyl acetate in heptane