反应详情

温度

20 °C

To a stirred solution of benzoylbenzaldehyde (2 g, 10 mmol) and 1,2-bis-(trimethoxysiloxy)ethane (2.3 g, 11 mmol) in dry dichloromethane (30 cm3) under N2 at room temperature was added trimethylsilylmethyl trifluoromethanesulphonate (5 drops). After stirring at 20° C. for 48 hours, pyridine (3 drops) was added followed by saturated NaHCO3 (20 cm3) and diethyl ether (20 cm3). The resulting mixture was stirred for 30 minutes. The ethereal layer was separated off and the aqueous layer extracted twice more with diethyl ether. The combined extracts were washed with water, dried over a mixture of anhydrous Na2CO3 and anhydrous Na2SO4 (1:1) and the solvent removed in vacuo to give 2-(3-benzoylphenyl)-1,3-dioxolane, nD20 1.5890. Yield 2.2 g (91.7%).

1. stirringThe resulting mixture was stirred for 30 minutes
2. customThe ethereal layer was separated off
3. extractionthe aqueous layer extracted twice more with diethyl ether
4. washThe combined extracts were washed with water
5. dry with materialdried over a mixture of anhydrous Na2CO3 and anhydrous Na2SO4 (1:1)
6. customthe solvent removed in vacuo