Hydrochloric Acid → HCID 67342805, compound

Participants

Reaction Steps

2.5 mL of methylene chloride, 0.015 mL of N,N-dimethylformamide and 0.095 mL of oxalyl chloride were added to 0.17 g of 3-cyanobenzoic acid at room temperature sequentially and stirred at the same temperature for 30 minutes. The reaction mixture was added to a mixed solution of 2.0 mL of methylene chloride and 0.35 mL of triethylamine containing 0.25 g of tert-butyl 2-amino-4-phenylbenzoate at room temperature and stirred at the same temperature for 10 minutes. Ethyl acetate, 1.0 mol/L hydrochloric acid and tetrahydrofuran were added to the reaction mixture. The organic layer was separated and dried over anhydrous magnesium sulfate after washed with a saturated sodium chloride aqueous solution, and the solvent was evaporated under reduced pressure. The obtained residue was purified with silica gel column chromatography [PSQ100B (spherical) manufactured by Fuji Silysia Chemical Ltd., eluent; chloroform] to obtain 0.29 g of tert-butyl 2-(3-cyanobenzamido)-4-phenylbenzoate as white solid.

Provenance & Evidence