反应详情

To a mixture of 1.2 g of sodium hydride and 0.1 mL of methanol in 50 mL of THF was added a solution of 10 g of 1,1-diphenyl-10-undecen-1-ol in 20 mL of THF over 2 hrs. The mixture was stirred at room temperature for 4 hrs, then 3.5 mL of dimethylsulfate was added. The mixture was stirred for an additional 75 hrs, then 2 mL of methanol was added to quench any excess sodium hydride. The solvent was distilled in vacuo, the residue taken up in ether, and the solution washed with 10% by wt of hydrochloric acid, water, and saturated sodium hydrogen carbonate. The solution was then dried with sodium sulfate and concentrated in vacuo to give 10.6 g of 11,11-diphenyl-11-methoxyundec-1-ene which is characterized by:

1. stirringThe mixture was stirred for an additional 75 hrs
2. customto quench any excess sodium hydride
3. distillationThe solvent was distilled in vacuo
4. washthe solution washed with 10% by wt of hydrochloric acid, water, and saturated sodium hydrogen carbonate
5. dry with materialThe solution was then dried with sodium sulfate
6. concentrationconcentrated in vacuo