反应详情

To a mixture of methyl 3-(4-chlorophenyl)-2-phenylpropionate (Step A, 20 g, 74 mmol) in acetonitrile (100 mL) and water (100 mL) was added lithium hydroxide monohydrate (8.8 g, 0.21 mol). After stirring at room temperature for 3 days, the volatile materials were removed by concentrating on a rotary evaporator and the residue was partitioned between water (300 mL) and hexane/ether (1:1, 200 mL). The water layer was separated, acidified to pH=2-3, and extracted with ethyl acetate (2×200 mL) The combined organic extracts were dried over anhydrous sodium sulfate, filtered, and concentrated to dryness to give the title compound. 1H NMR (500 MHz, CD3OD): δ 7.34-7.10 (m, 9H), 3.82 (dd, 1H), 3.36 (dd, 1H), 2.98 (dd, 1H).

1. customthe volatile materials were removed
2. concentrationby concentrating on a rotary evaporator
3. customthe residue was partitioned between water (300 mL) and hexane/ether (1:1, 200 mL)
4. customThe water layer was separated
5. extractionextracted with ethyl acetate (2×200 mL) The combined organic extracts
6. dry with materialwere dried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated to dryness