反应详情

温度

-60 °C

5.0 g (0.036 mol) of 4-isopropenylcyclohexanone (precursor to Example 4) were placed under inert gas in 150 ml of hexane, and 16.5 g (0.134 mol) of diethylzinc (1M in hexane) followed by 58.0 g (0.22 mol) of diiodomethane were added dropwise at -20° C. The mixture was stirred at -60° C. for 2 hours and then at 0° C. for 6 hours. The reaction solution was kept in a refrigerator overnight and was worked up by pouring it into cold NH4Cl solution and carrying out extraction with ether. The organic phase was washed with sodium thiosulfate solution and water, dried and concentrated. 5.3 g (96% of theory) of a colorless oil were obtained which was reacted without further purification.

1. additionwere added dropwise at -20° C
2. waitat 0° C. for 6 hours
3. customwas kept in a refrigerator overnight
4. extractionextraction with ether
5. washThe organic phase was washed with sodium thiosulfate solution and water
6. customdried
7. concentrationconcentrated
8. custom5.3 g (96% of theory) of a colorless oil were obtained which
9. customwas reacted without further purification