反应详情

To a stirred solution of 2-chlorophenol (10.0 g, 77.8 mmol) in carbon disulfide (20 ml) was added aluminum chloride (21.8 g, 163.4 mmol) at 0° C. under nitrogen. Acetyl chloride (6.72 g, 85.6 mmol) was added, and the mixture was heated at reflux temperature for 6 hours. The mixture was cooled down to room temperature, and poured into ice-water. The whole was extracted with diethylether. The organic layer was washed with brine, dried over MgSO4, and concentrated in vacuo. The residue was recrystallized with diethylether-hexane to give the title compound (6.39 g, 48% yield).

1. temperaturethe mixture was heated
2. temperatureat reflux temperature for 6 hours
3. extractionThe whole was extracted with diethylether
4. washThe organic layer was washed with brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. customThe residue was recrystallized with diethylether-hexane