反应详情

To the solution of 5-amino-1-[2,6-dichloro-4-(trifluoromethyl)phenyl]-4-formyl-1H-pyrazole-3-carbonitrile (0.5 g, 1.4 mmol) in dichloromethane (10 mL) was added N-bromosuccinimide (0.075 g, 0.2 mmol) followed by the addition of 1,3-dimercaptopropane (0.19 g, 1.8 mmol). The resulting solution was stirred at room temperature for eight hours. It was then worked-up by the addition of 2 N sodium hydroxide. The layers were separated and the organic layer was dried (Na2SO4) and concentrated. The resulting solid was further purified via silica gel column eluting with heptane:ethyl acetate (1:1) to afford a white solid (0.2 g, 33%). 19F-NMR: −64.231.

1. customThe layers were separated
2. dry with materialthe organic layer was dried (Na2SO4)
3. concentrationconcentrated
4. customThe resulting solid was further purified via silica gel column
5. washeluting with heptane:ethyl acetate (1:1)