2-[(4-methoxyphenyl)amino]-5-nitrobenzonitrile synthesis

Yield:85020-89-9 70%

Reaction Conditions:

with triethylamine in dimethyl sulfoxide at 100; for 40 h;Inert atmosphere;

Steps:

4.1

The first step reaction: Under nitrogen, to a 250mL three-necked flask equipped with a magnetic stirrer, thermometer and condenser, add 12.3g (100.0mmoL) of p-methoxyaniline, 10.2g (50.0mmoL) Fluoro-5nitrobenzonitrile, 10.1g (100.0mmoL) of triethylamine, add 48mL of dimethyl sulfoxide, under stirring, under nitrogen protection, react at 100 ° C for 40h; after cooling to room temperature, the material is discharged on ice Stir well in the water mixture, filter the resulting crude product and recrystallize with N, N-dimethylacetamide and ethanol (volume ratio 2: 1) to obtain 9.4 g of orange (2-cyano-4-nitro) -(4'-methoxy) -diphenylamine crystals, yield 70%, purity 97%;

References:

CN110903202,2020,A Location in patent:Paragraph 0121