反应详情

温度

60 °C

In a solution of 0.18 g of sodium cyanide and 0.29 g of ammonium chloride in 5 mL of 28% ammonia water, a solution of 1.0 g of 2-chloro-4-[5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydro-isoxazol-3-yl]benzaldehyde synthesized in Step 6 of Synthetic Example 6 in 30 mL of methanol was added, and stirred at 60° C. for 2 hours. After the completion of the reaction, the reaction mixture was left and cooled to room temperature, diluted with 60 mL of ethyl acetate, washed with water (30 mL×2), and the organic phase was dehydrated with and dried over saturated sodium chloride aqueous solution and anhydrous magnesium sulfate in that order, and the solvent was distilled off under reduced pressure to obtain 1.10 g of the aimed product as pale brown resinous substance.

1. customAfter the completion of the reaction
2. waitthe reaction mixture was left
3. temperaturecooled to room temperature
4. washwashed with water (30 mL×2)
5. dry with materialdried over saturated sodium chloride aqueous solution and anhydrous magnesium sulfate in that order
6. distillationthe solvent was distilled off under reduced pressure