2463-16-3

64-17-5

24964-64-5

2463-16-3

General procedure for the synthesis of ethyl 3-cyanobenzoate from ethanol and 3-cyanobenzaldehyde: A mixture of chlorobrominated resin and K2CO3 in MeOH-H2O (8:2, 3 mL) was placed in a round-bottomed flask equipped with a magnetic stirrer. 3-Cyanobenzaldehyde (1 mmol, 1 eq.) was added dropwise to the reaction system and the reaction mixture was continuously stirred at room temperature. The reaction process was monitored by thin layer chromatography (TLC). After completion of the reaction, the reaction mixture was filtered and the filtrate was extracted with ether (Et2O). The separated ether layer was washed sequentially with water and saturated brine and subsequently dried with anhydrous sodium sulfate (Na2SO4). The dried organic phase was filtered and concentrated to give the crude product. For further purification, the residue can be purified by silica gel column chromatography (60-120 mesh) using a mixture of petroleum ether (PE) and ethyl acetate (EtOAc) (9:1) as eluent.