反应详情

温度

67.5 °C

To 5-amino-3-cyano-4-(cyclohept-2-enyl)-1-(2,6-dichloro-4-trifluoromethylphenyl)-pyrazole (208 mg, 0.5 mmol, Example 10) in dry THF (8 ml) heated at 65° C. was added dropwise tert-butyl nitrite (160 mg, 1.5 mmol) in dry THF (2 ml) over 30 min. The solution was heated for a further 2 hr at 65-70° C. The solvent was removed in vacuo and the resulting brown oil purified by silica chromatography (eluting with hexane, hexane/diethyl ether 19/1, hexane/diethyl ether 9/1, hexane/diethyl ether 4/1, hexaneldiethyl ether 1/1, finally diethyl ether). The resulting orange solid was recrystallised from hexane to yield 80 mg of the title compound as a cream solid.

1. customThe solvent was removed in vacuo
2. customthe resulting brown oil purified by silica chromatography (
3. washeluting with hexane, hexane/diethyl ether 19/1, hexane/diethyl ether 9/1, hexane/diethyl ether 4/1, hexaneldiethyl ether 1/1, finally diethyl ether)
4. customThe resulting orange solid was recrystallised from hexane