反应详情

温度

70 °C

In a solution of 10.6 g of 3-chloro-4-methylbenzaldoxime in 60 mL of 1,2-dimethoxyethane, 9.2 g of N-chlorosuccinimide was added, and stirred at 70° C. for 2 hours. Then, the reaction mixture was left and cooled to room temperature, 11.3 g of 3,5-dichloro-1-(1-trifluoromethylethenyl)benzene synthesized in Step 1 of Synthetic Example 1, 15.6 g of potassium hydrogen carbonate and 10 mL of water were added, and continued to stir at room temperature further for 20 hours. After the completion of the reaction, the reaction mixture was diluted with 70 mL of ethyl acetate, washed with water (50 mL×1), and dehydrated with and dried over saturated sodium chloride aqueous solution and anhydrous sodium sulfate in that order, and then the solvent was distilled off under reduced pressure. The residual solid was washed with diisopropyl ether to obtain 13.8 g of the aimed product as white crystal.

1. waitThen, the reaction mixture was left
2. temperaturecooled to room temperature
3. stirringto stir at room temperature further for 20 hours
4. customAfter the completion of the reaction
5. washwashed with water (50 mL×1)
6. dry with materialdried over saturated sodium chloride aqueous solution and anhydrous sodium sulfate in that order
7. distillationthe solvent was distilled off under reduced pressure
8. washThe residual solid was washed with diisopropyl ether