反应详情

温度

100 °C

Under an argon atmosphere, a stirred solution of 3-(4-methyl-1H-imidazol-1-yl)-5-(trifluoromethyl)benzenamine (0.99 g, 4.1 mmol) in dry toluene (40 mL) is treated with a solution of AlMe3 (5 mL of 2 M in toluene; 10 mmol) at 40° C. After 45 min, a solution of 6[[(1,1-dimethylethyl)diphenylsilyl]oxy]-1-naphthalenecarboxylic acid, methyl ester (1.64 g, 3.72 mmol) in dry toluene (15 mL) is added and the stirred mixture is heated at 100° C. for 90 min. The cooled mixture is then added to a saturated aqueous solution of NH4Cl and stirred for 30 min. The organic phase is separated, washed with brine, dried (Na2SO4) and solvent is evaporated off under reduced pressure to give a residue, which is purified by column chromatography (SiO2; hexane/ethyl acetate 1:1) to afford the title compound as a beige solid.

1. customThe organic phase is separated
2. washwashed with brine
3. dry with materialdried (Na2SO4) and solvent
4. customis evaporated off under reduced pressure
5. customto give a residue, which
6. customis purified by column chromatography (SiO2; hexane/ethyl acetate 1:1)