反应详情

To a solution, prepared as described in (a), of 6 mmol of lithium cyclohexylisopropylamide in abs. THF there are added dropwise, at -78° , first 2.3 ml (18 mmol) of trimethylchlorosilane and then 1.2 g (5 mmol) of isovaleric acid 1-cyclohexyl-3-buten-2-yl ester. The solution is maintained at -78° for 1 hour, heated to room temperature over a period of 11/2 hours and stirred at that temperature for 1 hour. The reaction mixture is cooled to 0°, hydrolysed by adding 0.5 ml of methanol, diluted with ether, washed with 1N HCl and brine, dried over MgSO4 and concentrated by evaporation in a rotary evaporator. The residue is distilled as described in a) and yields the same product.

1. customTo a solution, prepared
2. temperatureThe solution is maintained at -78° for 1 hour
3. temperatureThe reaction mixture is cooled to 0°
4. washwashed with 1N HCl and brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated by evaporation in a rotary evaporator
7. distillationThe residue is distilled
8. customyields the same product