N-(2-cyanophenyl)benzamide synthesis

Yield:40288-69-5 97.7%

Reaction Conditions:

with triethylamine in dichloromethane at 25; for 18 h;Temperature;

Steps:

1.S1-3.S1 Specifically, the following steps are included

S1: adding 100 mmol of the compound of the above formula (1) to an appropriate amount of the organic solvent dichloromethane in the reaction vessel,200 mmol of the compound of the above formula (2) and 150 mmol of triethylamine, and the reaction was stirred at 25 ° C for 18 hours; After the reaction is completed, The solvent is distilled off under reduced pressure, and the solvent is removed.Then add enough ethyl acetate to dissolve the residue.Then, an appropriate amount of saturated sodium hydrogencarbonate aqueous solution and an appropriate amount of saturated sodium chloride water are sequentially added for washing.Separating the organic layer and the water layer,After the aqueous layer was extracted with ethyl acetate for 3 times,The organic layers are combined (that is, the organic layer separated by washing and washing, and the organic layer obtained by ethyl acetate extraction),Dry with anhydrous Na2SO4,Vacuum distillation,The residue was eluted by flash column chromatography on silica gel (a mixture of petroleum ether and ethyl acetate in a volume ratio of 5:1).The eluent was collected and evaporated to remove the eluent.Thus obtaining a compound of the above formula (3) as a yellow solid in a yield of 97.7%

References:

CN108409673,2018,A Location in patent:Paragraph 0063; 0065-0068; 0074; 0076-0079; 0084; 0086-0089