反应详情

温度

80 °C

To the THF suspension of zinc (5.72 g, 2 eq.), methanesulfonic acid (25.6 μl, 0.01 eq.) was added, and then stirred at 80° C. for 10 min. Then, the THF solution of 2-(3-bromo-4-methoxy-phenyl)-2-methyl-propionitrile (10 g, 39.35 mmol) was added, followed by addition of bromoethyl acetate (11.07 ml, 1.6 eq.) over 1 hr. The mixture was further stirred for 30 min. To the reaction solution, 4 M hydrochloric acid was added, and stirred at room temperature overnight. After extraction with ethyl acetate, the organic layer was washed with brine and dried over sodium sulfate. The drying agent was removed by filtration and the residues obtained after concentration under reduced pressure were purified by silica gel column chromatography (ethyl acetate/hexane) to obtain the title compound (orange oily substance, 9.74 g, 72%).

1. additionwas added
2. stirringThe mixture was further stirred for 30 min
3. stirringstirred at room temperature overnight
4. extractionAfter extraction with ethyl acetate
5. washthe organic layer was washed with brine
6. dry with materialdried over sodium sulfate
7. customThe drying agent was removed by filtration
8. customthe residues obtained
9. concentrationafter concentration under reduced pressure
10. customwere purified by silica gel column chromatography (ethyl acetate/hexane)