Phosphorus oxychloride → HCID 59580177, 화합물

참여 물질

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반응 단계

A mixture of 0.3 g (0.8 mmol) 1-methyl-2-(2,4,6-tribromo-phenoxy)-ethylamine (compound Z1.193, prepared as described in example P7) and 0.15 g (0.9 mmol) 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid in 2 ml pyridine under a nitrogen atmosphere is cooled to 0° C. Phosphorus oxychloride (0.08 ml, 0.9 mmol) is added dropwise and the reaction mixture is stirred at 80° C. for 12 h. The reaction mixture is diluted with water and 3-times extracted with ethyl acetate. The combined ethyl acetate layers are washed with 1.5 N HCl, saturated NaHCO3, water and brine, dried over sodium sulphate and evaporated to dryness. The residue is purified by column chromatography (using 60-120 mesh-silica gel in hexane; eluent: ethyl acetate) to yield 0.12 g 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid [1-methyl-2-(2,4,6-tribromo-phenoxy)-ethyl]-amide (27% of theory) as a yellow solid.

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