Ethanamine, 2,2,2-trifluoro- → HCID 23634409, compound

Participants

Reaction Steps

In a solution of 0.32 g of 1,1′-carbonylbis-1H-imidazole in 7.0 mL of tetrahydrofuran, 0.20 g of 2,2,2-trifluoroethylamine was added, and stirred at room temperature for 1.5 hour. Then, in the reaction mixture, a solution of 0.39 g of 3-[4-(aminomethyl)phenyl]-5-(3,5-dichlorophenyl)-5-trifluoromethyl-4,5-dihydro-isoxazole synthesized in Step 6 of Synthetic Example 1 in 5.0 mL of tetrahydrofuran was added, and continued to stir at room temperature further for 2.5 hours. After the completion of the reaction, the reaction mixture was diluted with 20 mL of ethyl acetate, washed with water (15 mL×2), and 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. The residue was purified with medium pressure preparative liquid chromatography (medium pressure collection apparatus: YFLC-Wprep manufactured by Yamazen Corporation) that was eluted with ethyl acetate-hexane (gradient of 1:8 to 1:1) to obtain 0.43 g of the aimed products as colorless resinous substance.

Provenance & Evidence