反应详情

温度

140 °C

A mixture of N-methyl-N-(p-toluenesulfonyl)-2-chloro-6-fluorobenzohydrazonoyl chloride (2.25 g), 2-chloro-4-(5-trifluoromethylpyridine-2-yloxy)benzonitrile (1.88 g), anhydrous iron (III) chloride (1.07 g) and o-dichlorobenzene (5 ml) is stirred at an oil bath temperature of 140° C. for 30 minutes. After cooling, it is dissolved in chloroform (300 ml) and washed with dilute hydrochloric acid, dilute aqueous solution of sodium hydroxide and saline. Then, it is dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The concentrate is purified by silica gel column chromatography using mixed solvent of hexaneethyl acetate as eluent to give 1.54 g of desired compound (melting point: 139.0°-141.0° C.).

1. temperatureAfter cooling
2. washwashed with dilute hydrochloric acid, dilute aqueous solution of sodium hydroxide and saline
3. dry with materialThen, it is dried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe concentrate is purified by silica gel column chromatography
6. additionusing mixed solvent of hexaneethyl acetate as eluent