反应详情

温度

70 °C

To a solution of methyl 5-benzyloxy-6-(3-chlorobenzylcarbamoyl)-1-(2,2-dimethoxyethyl)-4-oxo-1,4-dihydropyridine-3-carboxylate (2.0 g) in tetrahydrofuran (20 ml)-methanol (10 ml) was added 4N aqueous lithium hydroxide solution (1.5 ml) and the mixture was stirred at 70° C. for 1 hr. The precipitated solid was removed by thin layer of celite and washed with methanol. The solvent was evaporated and 1N aqueous hydrochloric acid (6.5 ml) and water (50 ml) were added. The mixture was extracted twice with ethyl acetate (75 ml each). The ethyl acetate layer was dried, concentrated and crystallized from ethyl acetate-diisopropyl ether to give 5-benzyloxy-6-(3-chlorobenzylcarbamoyl)-1-(2,2-dimethoxyethyl)-4-oxo-1,4-dihydropyridine-3-carboxylic acid (1.2 g).

1. customThe precipitated solid was removed by thin layer of celite
2. washwashed with methanol
3. customThe solvent was evaporated
4. addition1N aqueous hydrochloric acid (6.5 ml) and water (50 ml) were added
5. extractionThe mixture was extracted twice with ethyl acetate (75 ml each)
6. dry with materialThe ethyl acetate layer was dried
7. concentrationconcentrated
8. customcrystallized from ethyl acetate-diisopropyl ether