反应详情

温度

65 °C

To a mixture of toluene-4-sulfonic acid 2-[1-(4-methoxy-benzyl)-3-methyl-2-oxo-imidazolidin-4-yl]-ethyl ester (0.100 g, 0.239 mmole) and 2-(4-hydroxy-2-methyl-phenoxy)-2-methyl-propionic acid ethyl ester (0.063 g, 0.262 mmole) in anhydrous DMF (2.0 mL), is added cesium carbonate (0.093 g, 0.287 mmole). After heating at 65° C. for about 16 hours, the reaction mixture is partitioned between ethyl acetate (5 ml) and 1.0 N HCl aq. (5 ml), the aqueous layer is extracted with more ethyl acetate (2×5 ml). The combined organic layer is washed with brine (3×5 ml). The organic layer is dried over Na2SO4, filtered, and concentrated in vacuo. Chromatography using silica gel (0-40% acetone/hexane) produces a colorless oil (0.107 g, 91%). Mass [EI+] 485 (M+H)+.

1. customthe reaction mixture is partitioned between ethyl acetate (5 ml) and 1.0 N HCl aq. (5 ml)
2. extractionthe aqueous layer is extracted with more ethyl acetate (2×5 ml)
3. washThe combined organic layer is washed with brine (3×5 ml)
4. dry with materialThe organic layer is dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo