反应详情

4-bromomethyl-4′-nitrobenzophenone (3.20 g, 10.0 mmol, 1 eq) was dissolved in a 2:1 acetonitrile/water mixture (300 mL) and calcium carbonate (3.00 g, 30.0 mmol, 3 eq) was added. The turbid mixture was stirred under reflux for 60 hr. After this time the reaction mixture was allowed to cool and the solid calcium carbonate was filtered off. The solid was washed with ethyl acetate (10 mL) and the filtrate was concentrated under reduced pressure to give an off-white solid. The solid was dissolved in ethyl acetate and washed with concentrated hydrochloric acid. The organic solution was then neutralised with sodium bicarbonate, dried over magnesium sulfate and concentrated under reduced pressure to give 4-hydroxymethyl-4′-nitrobenzophenone (2.08 g, 81%) as a beige solid.

1. additionwas added
2. temperatureunder reflux for 60 hr
3. temperatureto cool
4. filtrationthe solid calcium carbonate was filtered off
5. washThe solid was washed with ethyl acetate (10 mL)
6. concentrationthe filtrate was concentrated under reduced pressure
7. customto give an off-white solid
8. washwashed with concentrated hydrochloric acid
9. dry with materialdried over magnesium sulfate
10. concentrationconcentrated under reduced pressure