反应详情

温度

60 °C

In a 50 ml dry three-neck-flask 1.5 g (7.6 mmol) of 4-hydroxy-benzophenone are suspended in 25 ml of 1,2-dichloroethane and heated to reflux under argon flow. 2.7 g (8.4 mmol) of tri-n-butylmethoxy tin are added to the solution in the course of 0.5 h. The conversion is complete according to the 1H-NMR-spectrum. The solution is concentrated and dried in high vacuum. 4.1 g of an orange oil crystallize. The crude product is dissolved at 90° C. in 20 ml of heptane. The solution is cooled and at about 60° C. brown crystals begin to form. After filtration, further cooling and freezing, the formation of crystals continues. The crystals are filtered, dried and analyzed. The structure is confirmed by 1H-NMR and 13C-NMR spectra. 3.0 g of the title product are obtained, melting at 76-82° C.

1. temperatureheated
2. temperatureto reflux under argon flow
3. concentrationThe solution is concentrated
4. customdried in high vacuum
5. custom4.1 g of an orange oil crystallize
6. dissolutionThe crude product is dissolved at 90° C. in 20 ml of heptane
7. customto form
8. filtrationAfter filtration
9. temperaturefurther cooling
10. filtrationThe crystals are filtered
11. customdried