反应详情

温度

130 °C

To a stirred solution of N-[1-fluoromethyl-2-(2,4,6-trichloro-phenyl)-ethyl]-O-methylhydroxylamine (0.20 g; 0.70 mmol), prepared as described in example P6f2 in chlorobenzene (3.8 ml) was added 2,6-lutidine (85 μl; 0.74 mmol) and 5-fluoro-1,3-dimethyl-1H-pyrazole-4-carbonyl fluoride (0.11 g; 0.70 mmol). The yellow solution was stirred at reflux (130° C.) for 22 hours. The dark brown solution was dissolved in dichloromethane (20 ml), washed with 1 M sodium hydroxide solution (20 ml), 1 M hydrochloric acid solution (20 ml), brine (20 ml), dried over sodium sulfate and evaporated under reduced pressure. The crude was subject to flash chromatography (eluant: c-hexane/ethyl acetate 9:1 to 7:3) to afford 20 mg (7% of theory) of 5-fluoro-1,3-dimethyl-1H-pyrazole-4-carboxylic acid [1-fluoromethyl-2-(2,4,6-trichlorophenyl)-ethyl]-methoxy-amide as a brown oil.

1. washwashed with 1 M sodium hydroxide solution (20 ml), 1 M hydrochloric acid solution (20 ml), brine (20 ml)
2. dry with materialdried over sodium sulfate
3. customevaporated under reduced pressure