反应详情

The compound ([5]-(53)-75) (7.60 g) prepared in Example 61 was dissolved in anhydrous chloroform (152 ml). Then, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (6.37 g), 1-hydroxybenzotriazole (4.48 g), and morpholine (6.31 g) were added to the solution. The reaction mixture was stirred at room temperature for 7 hours. After the reaction was completed, chloroform was added. The solution was washed with 0.5N HCl aqueous solution, 0.5N NaOH aqueous solution, and distilled water. After the organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (Kieselgel 60=150 g, hexane/ethyl acetate=1/1) to obtain the above-captioned compound ([5]-(54)-75) (8.50 g) as a white solid.

1. washThe solution was washed with 0.5N HCl aqueous solution, 0.5N NaOH aqueous solution
2. distillationdistilled water
3. dry with materialAfter the organic layer was dried over anhydrous sodium sulfate
4. customthe solvent was evaporated under reduced pressure
5. customthe residue was purified by silica gel column chromatography (Kieselgel 60=150 g, hexane/ethyl acetate=1/1)