反应详情

In a 50 ml dry three-neck-flask, 2.0 g (8.8 mmol) 4-benzoylbenzoic acid in 30 ml 1,2-dichlorethane are suspended under argon flow and heated to reflux. 2.8 g (8.8 mmol) tri-n-butylmethoxy tin are added slowly in the course of 0.5 h. The conversion is complete according to the 1H-NMR-spectrum. The slightly turbid hot solution is filtered, cooled and concentrated. 3.6 g of the crude product are obtained as yellowish oil. 2.4 g thereof are heated in a bulb-to-bulb distillation apparatus (0.03 mbar) and distilled at 190° C. 1.9 g of the title product is obtained as colorless oil. The structure is confirmed by 1H-NMR and 13C-NMR-spectra.

1. customIn a 50 ml dry three-neck-flask
2. temperatureheated to reflux
3. filtrationThe slightly turbid hot solution is filtered
4. temperaturecooled
5. concentrationconcentrated
6. custom3.6 g of the crude product are obtained as yellowish oil
7. temperature2.4 g thereof are heated in a bulb-to-bulb distillation apparatus (0.03 mbar)
8. distillationdistilled at 190° C