反应详情

To a solution of ethyl 4-bromo-3-oxocyclohexanecarboxylate (3.73 g, 15 mmol) in EtOH (30 mL) at 80° C. was added a solution of benzenethiol (1.65 mL, 15 mmol) and NaOH (0.6 g, 15 mmol) in EtOH (100 mL). The suspension was stirred for 1 hour, then was concentrated in vacuo. The residue was diluted with water and extracted with EtOAc. The organic layer was washed with water then brine, then was dried over MgSO4 and concentrated in vacuo. Purification by chromatography on silica gel afforded 2.56 g (61%) of the title compound as a yellow oil: MS (−) 277 (M−H)−.

1. concentrationwas concentrated in vacuo
2. additionThe residue was diluted with water
3. extractionextracted with EtOAc
4. washThe organic layer was washed with water
5. dry with materialbrine, then was dried over MgSO4
6. concentrationconcentrated in vacuo
7. customPurification by chromatography on silica gel