反应详情

温度

80 °C

Into a 500 mL flask was weighed 25.0 g (139.6 mmol) of 2-chlorophenylhydrazine hydrochloride, 27.4 g (153 mmol) of 4,4,4-trifluoro-1-furan-2-yl-butane-1,3-dione, and 200 mL of acetic acid. The resulting solution was heated at 80° C. for 18 h then was cooled and was washed into a separatory funnel with 1.0 M NaOH and ethyl acetate. The ethyl acetate was separated, washed with 1.0 M NaOH, brine, dried (Na2SO4), and was concentrated in vacuo. The residue was filtered through a short column of silica gel affording 1-(2-chlorophenyl)-5-furan-2-yl-3-trifluoromethyl-1H-pyrazole as a brown oil, yield: 37.31 g (85%); MS (ES): 313 [M+H]+.

1. customInto a 500 mL flask was weighed
2. temperaturethen was cooled
3. washwas washed into a separatory funnel with 1.0 M NaOH and ethyl acetate
4. customThe ethyl acetate was separated
5. washwashed with 1.0 M NaOH, brine
6. dry with materialdried (Na2SO4)
7. concentrationwas concentrated in vacuo
8. filtrationThe residue was filtered through a short column of silica gel