反应详情

温度

0 °C

A solution of syringic acid (20 mg) in dry DMF (2 ml) was cooled to 0° C. 1-Ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (WSCI) and 1-hydroxybenztriazole hydrate (HOBt) were added thereto in that order. The mixture was stirred at 0° C. for one hr. The compound (30 mg) obtained in step (e) of Example 1 and triethylamine were added thereto in that order. The mixture was stirred at 0° C. for one hr, and then stirred at room temperature overnight. A saturated aqueous ammonium chloride solution(5 ml) was added thereto, followed by separation with ethyl acetate and water. The ethyl acetate layer was washed with an aqueous sodium chloride solution, dried over magnesium sulfate, and then concentrated under the reduced pressure. The residue was purified by chromatography on silica gel (chloroform:methanol=20:1) to give 42 mg of the title compound.

1. stirringThe mixture was stirred at 0° C. for one hr
2. stirringstirred at room temperature overnight
3. customfollowed by separation with ethyl acetate and water
4. washThe ethyl acetate layer was washed with an aqueous sodium chloride solution
5. dry with materialdried over magnesium sulfate
6. concentrationconcentrated under the reduced pressure
7. customThe residue was purified by chromatography on silica gel (chloroform:methanol=20:1)