反应详情

The compound (146 mg, 0.60 mmol) obtained in Step 2 of Reference Example 13, triethylamine (0.14 ml, 1.00 mmol), 1-hydroxybenzotriazole (74 mg, 0.55 mmol), and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (105 mg, 0.55 mmol) were added to an N,N-dimethylformamide (5 ml) solution of the compound (246 mg, 0.50 mmol) obtained in Step 1 above and the resulting mixture was stirred at room temperature for 18 hours. The reaction mixture was diluted with ethyl acetate, washed with water, saturated sodium bicarbonate solution, and brine in that order and then dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, then the residue was purified by silica gel column chromatography [chloroform:methanol=70:1 (v/v)] and the purified product obtained was dissolved in methanol (10 ml) and stirred at 60° C. for 24 hours. The solvent was evaporated under reduced pressure to give 150 mg (47%) of the title compound as a pale yellow solid.

1. washwashed with water, saturated sodium bicarbonate solution, and brine in that order
2. dry with materialdried over anhydrous sodium sulfate
3. customThe solvent was evaporated under reduced pressure
4. customthe residue was purified by silica gel column chromatography [chloroform:methanol=70:1 (v/v)]
5. customthe purified product obtained
6. stirringstirred at 60° C. for 24 hours
7. customThe solvent was evaporated under reduced pressure