反应详情

温度

20 °C

A solution of trimethylaluminium in toluene (10 mL of 2.0 M) is added over 30 minutes to a stirred suspension of ammonium choride (1.07 g, 20 mmol) in toluene (20 mL) at 5° C. under an argon atmosphere. The mixture is stirred at 20° C. for 2 h, treated with a solution of 4'-methoxy-3'-(3-nitrophenyl)-[1,1'-biphenyl]-4-carboxylic acid, ethyl ester (1.65 g, 4.3 mmol) in toluene (40 mL) and stirred at 60° C. for 18 h. The cooled mixture is washed with hydrochloric acid (50 mL of 0.5 M) followed by saturated aqueous sodium chloride (50 mL), dried (Na2SO4). filtered and the solvent is evaporated off under reduced pressure to yield the crude product which is purified by crystallisation from ethyl acetate-t-butylethyl ether to give 4'-methoxy-3'-(3-nitrophenyl)-[1,1'-biphenyl]-4-carboxamide as a colourless crystalline solid, m.p. 201-205° C.

1. stirringstirred at 60° C. for 18 h
2. washThe cooled mixture is washed with hydrochloric acid (50 mL of 0.5 M)
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. customthe solvent is evaporated off under reduced pressure
6. customto yield the crude product which
7. customis purified by crystallisation from ethyl acetate-t-butylethyl ether