反应详情

温度

40 °C

To a solution of 1-(2,6-dichloro-4-trifluoromethylphenyl)-3-cyano-5-(2-methoxyethylamino)-4-trifluoromethylsulfonylpyrazole (1.5g, 2.9 mmol) in tetrahydrofuran at 20° C. under nitrogen, was added sodium hydride (0.38 g, 60% in oil, 9.4 mmol), and stirred for 0.5 hour. Iodomethane (1.68 g, 11.7 mmol) was added and the mixture stirred for 15 hours at 20° C., then heated to 40° C. for 8 hours. The mixture was added to ethyl acetate and saturated ammonium chloride solution. The organic layer was washed with water and brine, dried (sodium sulfate), evaporated and chromatographed on silica gel eluting with heptane-ethyl acetate (9:1) to give 1-(2,6-dichloro-4-trifluoromethylphenyl-3-cyano-5-[N-(2-methoxyethyl)-N-methylamino]-4-trifluoromethylsulfonylpyrazole as a white solid (Compound number 2-3, 0.78 g), mp 75° C.

1. stirringthe mixture stirred for 15 hours at 20° C.
2. washThe organic layer was washed with water and brine
3. dry with materialdried (sodium sulfate)
4. customevaporated
5. customchromatographed on silica gel eluting with heptane-ethyl acetate (9:1)