反应详情

To a solution of 4-carboxybenzaldehyde (1.06 g) in chloroform (14.1 mL), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (2.03 g), 1-hydroxybenzotriazole monohydrate (1.62 g) and piperdine (1.05 mL) were added. After stirring the mixture at room temperature for 15 hours, a saturated aqueous solution of ammonium chloride was added. After extraction with ethyl acetate, the combined organic layers were washed with saturated brine. The washed organic layers were dried over anhydrous magnesium sulfate and after removing the desiccant by filtration, the filtrate was concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=85:15-30:70) to give the titled compound as a colorless oil (1.57 g).

1. extractionAfter extraction with ethyl acetate
2. washthe combined organic layers were washed with saturated brine
3. dry with materialThe washed organic layers were dried over anhydrous magnesium sulfate
4. customafter removing the
5. filtrationdesiccant by filtration
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe resulting residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=85:15-30:70)