反应详情

温度

100 °C

To 10 ml of anhydrous DMF were added 2.8 g of N- Boc-p-hydroxyphenylglycine methyl ester and 1.38 g (1.0 eq) of anhydrous potassium carbonate, followed by addition of 2.68 g (1.0 eq.) of N-(3-bromopropyl)phthalimide. The mixture was heated at 100° C. for 1 hour. The reaction mixture was poured into ice water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride, and dried. Thereafter, the solvent was distilled off. The residue was purified by silica gel column chromatography (eluent: 5% ethyl acetate/dichloromethane), to give colorless crystals.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed with water
3. dry with materiala saturated aqueous solution of sodium chloride, and dried
4. distillationThereafter, the solvent was distilled off
5. customThe residue was purified by silica gel column chromatography (eluent: 5% ethyl acetate/dichloromethane)
6. customto give colorless crystals