反应详情

A 1.0 mol/L tetrabutylammonium fluoride-tetrahydrofuran solution (0.56 mL) was added to a tetrahydrofuran (3.2 mL) solution of the obtained tert-butyl 2-(2-(benzyloxy)-5-(4-(tert-butyldimethylsilyloxy)piperidin-1-yl)benzamido)-4-phenylbenzoate (0.32 g), followed by stirring at room temperature for 1 hour. A 1.0 mol/L tetrabutylammonium fluoride-tetrahydrofuran solution (0.28 mL) was added to the reaction mixture, followed by stirring at room temperature for 4 hours. Water was added to the reaction mixture under ice-cooling, and chloroform was added thereto at room temperature. The organic layer was separated, washed with a saturated aqueous solution of sodium chloride, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography [eluent: 90-40% hexane/ethyl acetate] to obtain 0.23 g of tert-butyl 2-(2-(benzyloxy)-5-(4-hydroxypiperidin-1-yl)benzamido)-4-phenylbenzoate.

1. stirringby stirring at room temperature for 4 hours
2. temperaturecooling
3. customat room temperature
4. customThe organic layer was separated
5. washwashed with a saturated aqueous solution of sodium chloride
6. dry with materialdried over anhydrous magnesium sulfate
7. customthe solvent was evaporated under reduced pressure
8. customThe obtained residue was purified by silica gel column chromatography [eluent: 90-40% hexane/ethyl acetate]