反应详情

2.3 g (19.5 mmol) Potassium tert-butoxide is dissolved in 500 mL dry THF, and 7.18 g (37 mmol) tetraethylene glycol is added dropwise. After stirring for 30 min, a solution of 3.31 g (19.7 mmol) allyl iodide in 60 mL dry THF is added over 1 h, and stirring is continued for 24 h. The crude mixture is filtered over silica gel and the solvent removed in vacuo. The product is purified by silica gel chromatography (gradient: petrol ether/ethyl acetate 10:1→ethyl acetate), yielding 2.41 g 22 (10.3 mmol, 27%) as a colorless liquid.

1. stirringstirring
2. waitis continued for 24 h
3. filtrationThe crude mixture is filtered over silica gel
4. customthe solvent removed in vacuo
5. customThe product is purified by silica gel chromatography (gradient: petrol ether/ethyl acetate 10:1→ethyl acetate)