1,2-Dichloroethane → HCID 86761701, compound

Participants

Reaction Steps

To a solution of 3.56 g of 5-[3-bromo-5-(trifluoromethyl)phenyl]-3-(3-chloro-4-methylphenyl)-5-trifluoromethyl-4,5-dihydroisoxazole in 15 mL of 1,2-dichloroethane, 1.43 g of N-bromosuccinimide and 0.096 g of α,α′-azobisisobutyronitrile were added and the resultant mixture was stirred while heating the reaction mixture to reflux for 3 hours. After the completion of the reaction, the reaction mixture was left to be cooled down to room temperature and 50 mL of 1,2-dichloroethane was added to the reaction mixture. Subsequently, the resultant mixture was washed with water (30 mL×1) and then dehydrated and dried over saturated saline and anhydrous sodium sulfate in this order, and the solvent was distilled off under reduced pressure. The resultant residue was dissolved in 7 mL of an N,N-dimethylformamide solution, and 1.35 g of a phthalimide potassium salt was added to the resultant solution, followed by stirring the resultant mixture at room temperature for 1 hour. After the completion of the reaction, the reaction mixture was charged into 30 mL of water and the resultant reaction mixture was extracted with ethyl acetate (25 mL×2). The organic phase was dehydrated and dried over saturated saline and anhydrous magnesium sulfate in this order, and the solvent was distilled off under reduced pressure to obtain 5.26 g of a crude objective substance as a light yellow resinoid. This substance was used in the next process as it was without being further purified.

Provenance & Evidence