反应详情

To a stirred solution of N-bromosuccinimide (1.11 g, 6.274 mmol), PTSA (0.108 g, 0.627 mmol) in toluene (15 mL) was added 4-oxocyclohexanecarboxylic acid ethyl ester (1.068 g, 6.274 mmol) under nitrogen atmosphere and the reaction was refluxed for 2 hrs. Toluene was evaporated under reduced pressure and the residue was partitioned between water (50 mL) and ethyl acetate (50 mL). The layers were separated; the organic layer was washed with sat. sodium bicarbonate solution followed by brine, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to get title the compound (2.2 g) which was carried without purification for the next step.

1. temperaturethe reaction was refluxed for 2 hrs
2. customToluene was evaporated under reduced pressure
3. customthe residue was partitioned between water (50 mL) and ethyl acetate (50 mL)
4. customThe layers were separated
5. washthe organic layer was washed with sat. sodium bicarbonate solution
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure