反应详情

温度

-78 °C

s-BuLi (28.0 mL, 1.3 M) was added slowly to a solution of Compound 20b (7.0 g) in THF (50 mL) at −78° C. The mixture stirred for 1 hr at −78° C. and then (2-chloro-ethyl)-benzene Compound 20c (5.11 g, 36.4 mmol) in THF (10 mL) was added dropwise. The reaction mixture was stirred for 24 hrs while warming to r.t. The reaction was quenched with 1N HCl (5 mL), then diluted with water (100 mL) and EtOAc (500 mL). The organic layer was washed with brine, separated and dried with anhydrous sodium sulfate, then filtered and concentrated in vacuo to yield a crude product. Purification by flash chromatography (eluted with 10% EtOAc in Hexane) afforded 2-phenethyl-cyclohexanone Compound 20d (4.05 g, 20.0 mMol, 58%) as a yellow oil.

1. stirringThe reaction mixture was stirred for 24 hrs
2. temperaturewhile warming to r.t
3. customThe reaction was quenched with 1N HCl (5 mL)
4. additiondiluted with water (100 mL) and EtOAc (500 mL)
5. washThe organic layer was washed with brine
6. customseparated
7. dry with materialdried with anhydrous sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated in vacuo
10. customto yield a crude product
11. customPurification
12. washby flash chromatography (eluted with 10% EtOAc in Hexane)