反应详情

温度

140 °C

A mixture of 1.30 g of N-methyl-N-phenylsulfonyl-2-chloro-6-fluorobenzohydrazonoyl chloride, 1.00 g of 4-(3-chloro-5-trifluoromethylpyridin-2-yloxy)benzonitrile, 0.50 g of anhydrous aluminum chloride and 3 ml of o-dichlorobenzene was stirred in an oil bath at a temperature of 140° C. for 30 minutes. After the cooling, the resulting solution was dissolved in 100 ml of chloroform, washed with diluted hydrochloric acid solution, diluted sodium hydroxide solution and saline water in this order, dried over anhydrous magnesium sulfate and concentrated under a reduced pressure. The resulting concentrate was purified through a chromatography of silica gel column using a mixed solution of hexane and ethyl acetate as a developing solvent to obtain 0.70 g of the given compound (measurement of nD20 was impossible). NMR data (60 MHz, CDCl3 solvent, δ value)

1. washwashed with diluted hydrochloric acid solution, diluted sodium hydroxide solution and saline water in this order
2. dry with materialdried over anhydrous magnesium sulfate
3. concentrationconcentrated under a reduced pressure
4. concentrationThe resulting concentrate
5. customwas purified through a chromatography of silica gel column