反应详情

To 3.1 g (25 mmol) 1-ethynyl-1-cyclohexanol in 25 ml acetonitrile were added 7.1 ml (75 mmol, 3 eq) acetic anhydride at −20° C. 12.3 mg (0.03 mmol) scandiumtriflate in 300 μl THF were added and the solution was stirred for 2 h. Additional 12.3 mg (0.03 mmol) scandiumtriflate in 300 μl THF were added and stirring was continued for 30 min. A saturated aqueous solution of NaHCO3 and ether were added. The layers were separated and the inorganic one was extracted with ether. The combined organic phases were washed with brine and dried over Na2SO4. Evaporation yielded 4.6 g crude 1-ethynylcyclohexyl acetate as colorless oil, MS: 166 (M).

1. stirringstirring
2. waitwas continued for 30 min
3. customThe layers were separated
4. extractionthe inorganic one was extracted with ether
5. washThe combined organic phases were washed with brine
6. dry with materialdried over Na2SO4
7. customEvaporation