反应详情

A solution of 60 g (0.47 mol) of cyclohexylacetaldehyde in 400 ml of abs. THF is added dropwise at -20° to a solution of vinylmagnesium bromide in abs. THF, prepared from 13.8 g (0.57 mol) of magnesium and 66.3 g (0.62 mol) of vinyl bromide in 500 ml of abs. THF. When the addition is complete, the whole is stirred for 30 minutes at -20° and then hydrolysed with 900 ml of saturated ammonium chloride solution. After diluting with 250 ml of H2O, the reaction mixture is extracted three times with 1 liter of ether each time, washed three times with 500 ml of brine each time, dried with MgSO4 and then concentrated by evaporation in a rotary evaporator. The residue is distilled at 50°/0.1 mbar.

1. additionWhen the addition
2. extractionthe reaction mixture is extracted three times with 1 liter of ether each time
3. washwashed three times with 500 ml of brine each time
4. dry with materialdried with MgSO4
5. concentrationconcentrated by evaporation in a rotary evaporator
6. distillationThe residue is distilled at 50°/0.1 mbar