反应详情

温度

140 °C

A mixture of N-methyl-N-(p-toluenesulfonyl)-2-chloro-6-fluorobenzohydrazonoyl chloride (7.50 g), 3-chloro-4-methylbenzonitrile (3.33 g), anhydrous aluminum chloride (3.00 g) and o-dichlorobenzene (20 ml) is stirred at an oil bath temperature of 140° C. for 1 hour. After cooling, it is washed with 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 hexane-ethyl acetate as eluent to give 3.70 g of desired compound.

1. temperatureAfter cooling
2. washit is washed with 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 hexane-ethyl acetate as eluent