反应详情

To a suspension of N-[(2,6-dichlorophenyl)carbonyl]-4-(1,3,6-trimethyl-2,4-dioxo-5-pyrimidinyl)-L-phenylalanine (0.6 mmol, 300 mg) and sodium bicarbonate (3.6 mmol, 302 mg) in DMF (4 mL) was added iodoethane (3.6 mmol, 0.29 mL) at room temperature. The mixture was stirred for 72 h at room temperature. Then, the reaction mixture was poured into water (50 mL) and was extracted with ethyl acetate (3×20 mL). The combined extracts were washed with brine solution (60 mL) and were dried over anhydrous magnesium sulfate. Filtration of the drying agent and concentration of the filtrate gave the crude product which was purified by silica gel chromatography using a Biotage (40m) column to obtain 155 mg (50% yield) of N-[(2,6-dichlorophenyl)carbonyl]-4-(1,3,6-trimethyl-2,4-dioxo-5-pyrimidinyl)-L-phenylalanine ethyl ester as a crystalline white solid: mp 262-265° C. ES-HRMS m/e calcd for C25H25Cl2N3O5 (M+Na) 540.1062, found 540.1049.

1. extractionwas extracted with ethyl acetate (3×20 mL)
2. washThe combined extracts were washed with brine solution (60 mL)
3. dry with materialwere dried over anhydrous magnesium sulfate
4. filtrationFiltration of the drying agent and concentration of the filtrate
5. customgave the crude product which
6. customwas purified by silica gel chromatography