反应详情

A mixture of 5.0 g (18.5 mmol) of 2-hydroxy-4-(2,3-epoxypropoxy)benzophenone and 15.0 g (58.7 mmol) of 1-cyclohexyloxy-4-hydroxy-2,2,6,6-tetramethylpiperidine is heated to 80° and then treated with 0.5 g of phosphorous acid (99%). The reaction mixture is heated at 80°-90° C. for 6 hours, then cooled and dissolved in ethyl acetate (200 ml). The organic solution is washed with saturated sodium bicarbonate solution (100 ml), dried over magnesium sulfate, and evaporated to a yellow oil. Purification by flash chromatography on silica gel to obtain the least polar material formed in the reaction mixture affords approximately 200 mg of the title compound, a yellow glass.

1. temperatureis heated to 80°
2. temperatureThe reaction mixture is heated at 80°-90° C. for 6 hours
3. temperaturecooled
4. washThe organic solution is washed with saturated sodium bicarbonate solution (100 ml)
5. dry with materialdried over magnesium sulfate
6. customevaporated to a yellow oil
7. customPurification by flash chromatography on silica gel
8. customto obtain the least polar material
9. customformed in the reaction mixture