反应详情

To a solution of N-butyl-N-[4′-(trifluoromethyl)-1,1′-biphenyl-3-yl]amine (73 mg, 0.25 mmol) in anhydrous acetonitrile (5 mL) was added ethyl [4-(bromomethyl)-2-methylphenoxy]acetate (75 mg, 0.25 mmol) and N,N-diisopropylethylamine (43 μL, 0.25 mmol). The resulting solution was heated at reflux under nitrogen for 2 h and then cooled to room temperature. The solvent was removed in vacuo and the residue diluted with water (10 mL) and extracted with CH2Cl2 (30 mL). The organic extract was separated by hydrophobic frit and the solvent removed in vacuo. Purification by SPE (Silica, 5 g) eluting 99:1 cyclohexane:EtOAc afforded the title compound as a pale yellow oil (105 mg).

1. temperatureThe resulting solution was heated
2. temperatureat reflux under nitrogen for 2 h
3. customThe solvent was removed in vacuo
4. additionthe residue diluted with water (10 mL)
5. extractionextracted with CH2Cl2 (30 mL)
6. extractionThe organic extract
7. customwas separated by hydrophobic frit
8. customthe solvent removed in vacuo
9. customPurification by SPE (Silica, 5 g)
10. washeluting 99:1 cyclohexane