反应详情

温度

65 °C

A mixture of 3-(3-hydroxy-phenyl)-2-methyl-2-phenoxy-propionic acid ethyl ester (0.100 g, 0.271 mmol), toluene-4-sulfonic acid 2-[3-methyl-2-oxo-1-(4-trifluoromethyl-benzyl)-imidazolidin-4-yl]-ethyl ester (0.136 g, 0.298 mmol) and Cs2CO3 (0.133 g, 0.408 mmol) in DMF (8 mL) was heated to 65° C. under N2 for 17 h. The reaction was cooled and quenched with 1 N HCl (10 mL) and worked up extractively with Et2O and water. The organic layer was dried (MgSO4) and the solvent removed in vacuo to afford crude product that was purified by flash chromatography using 4:1 hexanes:acetone to afford 0.113 g (64%) 2-methyl-3-(3-{2-[3-methyl-2-oxo-1-(4-trifluoromethyl-benzyl)-imidazolidin-4-yl]-ethoxy}-phenyl)-2-(4-trifluoromethyl-phenoxy)-propionic acid ethyl ester. 1H NMR. MS (ES+) Calc'd for C33H35N2O5F6 (M +1) 653. Found m/z 653 (100%).

1. temperatureThe reaction was cooled
2. customquenched with 1 N HCl (10 mL)
3. dry with materialThe organic layer was dried (MgSO4)
4. customthe solvent removed in vacuo
5. customto afford crude product that
6. customwas purified by flash chromatography