反应详情

To a stirred solution of 5-amino-1-(2,6-dichloro-4-trifluoromethylphenyl)-3-methyl 4-trimethylsilylethynylpyrazole (1.3 g) in tetrahydrofuran (15 ml) at 65° C. was added dropwise t-butylnitrite (1.65 g) in tetrahydrofuran (5 ml) over a period of 15 minutes and heating continued for 3 hours. The reaction mixture was left at room temperature overnight then evaporated to give the crude product as a gum which was purified by column chromatography on silica gel eluted with dichioromethane:hexane (1:1). Combination and evaporation of appropriate fractions provided the title compound as a pale yellow solid, m.p. 76-78° C.

1. temperatureheating
2. waitThe reaction mixture was left at room temperature overnight
3. customthen evaporated
4. customto give the crude product as a gum which
5. customwas purified by column chromatography on silica gel
6. washeluted with dichioromethane:hexane (1:1)
7. customCombination and evaporation of appropriate fractions