反应详情

To a solution of 4-[4-(morpholin-4-yl)-phenyl]semicarbazide (IM9-O-01:70.9 mg, 0.3 mmol) and 5-isopropyl-2,4-bis(methoxymethoxy)-benzoic acid (IM3-a:85.3 mg, 0.3 mmol) in dimethylformamide (4 mL), were added N-methylpyrrolidone (0.2 mL), 1-hydroxybenzotriazole monohydrate (60.8 mg, 0.45 mmol), and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide (115.0 mg, 0.6 mmol) successively, and the mixture was stirred at room temperature overnight. The reaction mixture was mixed with ethyl acetate (30 mL) and 5% aqueous sodium hydrogencarbonate (20 mL). The aqueous layer was separated, and extracted with ethyl acetate. The combined organic layers thus obtained were dried over anhydrous sodium sulfate. Sodium sulfate was removed by filtration, the solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (dichloromethane: methanol=30:1-20:1) to obtain the title compound (IM5-O-a01: colorless syrup, 104.9 mg, 70%).

1. customThe aqueous layer was separated
2. extractionextracted with ethyl acetate
3. customThe combined organic layers thus obtained
4. dry with materialwere dried over anhydrous sodium sulfate
5. customSodium sulfate was removed by filtration
6. distillationthe solvent was distilled off under reduced pressure
7. customthe residue was purified by silica gel column chromatography (dichloromethane: methanol=30:1-20:1)