反应详情

3-Adamantan-1-yl-4-hydroxybenzoic acid (0.286 g), N-hydroxysuccinimide (0.12 g) and N,N′-dicyclohexylcarbodiimide (0.22 g) are dissolved in dioxane (5 mL) and stirred for 12 hours. The produced solid is filtered and the filtrate is added dropwise to a mixture solution of 3,4-dihydroxybenzylamine bromate (0.25 g), sodium bicarbonate (0.09 g) and water (1 mL). After stirring at 50° C. for 2 hours, the solution is cooled to room temperature, neutralized with 10% HCl solution and washed with ethyl acetate (30 mL). The organic layer is dried with anhydrous magnesium sulfate, filtered, concentrated under reduced pressure and separated by column chromatography to obtain 0.03 g of the target compound as white solid.

1. filtrationThe produced solid is filtered
2. additionthe filtrate is added dropwise to a mixture solution of 3,4-dihydroxybenzylamine bromate (0.25 g), sodium bicarbonate (0.09 g) and water (1 mL)
3. stirringAfter stirring at 50° C. for 2 hours
4. washwashed with ethyl acetate (30 mL)
5. dry with materialThe organic layer is dried with anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. customseparated by column chromatography