反应详情

温度

20 °C

1-(Bromocyclohexyl)-4-nitrobenzene (18.4 g, 64.8 mmol), lithium carbonate (5.3 g, 71.2 mmol), and lithium bromide (6.2 g, 71.2 mmol) were reacted together in DMF (100 mL) for 2 hours at 160° C. The reaction mixture was cooled to 20° C., diluted with ethyl acetate (500 mL), and washed with water (300 mL). The aqueous phase was extracted with ethyl acetate (200 mL) and the combined organic phases were washed with water (3×150 mL), dried over MgSO4 and concentrated in vacuo. The residue was purified on silica (350 g) using ethyl acetate and heptane (1:9) as eluent to give 11.7 g of 1-cyclohex-1-enyl-4-nitrobenzene.

1. washwashed with water (300 mL)
2. extractionThe aqueous phase was extracted with ethyl acetate (200 mL)
3. washthe combined organic phases were washed with water (3×150 mL)
4. dry with materialdried over MgSO4
5. concentrationconcentrated in vacuo
6. customThe residue was purified on silica (350 g)