反应详情

温度

65 °C

A suspension of 2.0 g (14 mmol) of Ca(OCl)2, 1.38 g (10 mmol) of potassium carbonate and 0.40 g (7.12 mmol) of potassium hydroxide in 40 ml of water was stirred at 65° C. for 30 minutes and filtered. The filtrate was added to 0.53 g (2 mmol) of 3',5'-bis(trimethylsilyl)acetophenone and the mixture was refluxed for 7.5 hours with stirring. After cooling, 3 ml of aqueous sodium bisulfite solution was added to the reaction mixture. The aqueous solution was extracted with AcOEt. The extract was washed successively with water and sat.aq.NaCl, dried over anhyd.Na2SO4 and evaporated. The residue was purified by column chromatography on silica gel [eluent: n-hexane-AcOEt (2:1-1:1)] to give 0.27 g of white powder, m.p. >300° C. (yield 51%).

1. filtrationfiltered
2. temperaturethe mixture was refluxed for 7.5 hours
3. stirringwith stirring
4. temperatureAfter cooling
5. extractionThe aqueous solution was extracted with AcOEt
6. washThe extract was washed successively with water and sat.aq
7. dry with materialNaCl, dried over anhyd
8. customNa2SO4 and evaporated
9. customThe residue was purified by column chromatography on silica gel [eluent: n-hexane-AcOEt (2:1-1:1)]