反应详情

A mixture of 4.0 g (11.3 mmol) of methyl 3-(2H-benzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydrocinnamate and 8.0 g (28.1 mmol) of 4-amino-1-octyloxy-2,2,6,6-tetramethylpiperidine is heated at 190°-200° C. for 2 hours. The reaction mixture is dissolved in ethyl acetate (300 ml). The organic solution is washed with 1N hydrochloric acid (2 ×100 ml) and saturated sodium bicarbonate solution (200 ml), then dried over magnesium sulfate and evaporated to obtain a solid. Purification by flash chromatography on silica gel (3:1 heptane: ethyl acetate) following by recrystallization from methanol affords 1.0 g (15% yield) of the title compound, a white solid, mp 153°-9° C.

1. temperatureis heated at 190°-200° C. for 2 hours
2. washThe organic solution is washed with 1N hydrochloric acid (2 ×100 ml) and saturated sodium bicarbonate solution (200 ml)
3. dry with materialdried over magnesium sulfate
4. customevaporated
5. customto obtain a solid
6. customPurification by flash chromatography on silica gel (3:1 heptane: ethyl acetate)
7. customfollowing by recrystallization from methanol