反应详情

2.00 g (8.93 mmol) of Compound b obtained in Reference Example 2 was gently added to a suspension of 356 mg (8.93 mmol) of 60% sodium hydride in 20 ml of N,N-dimethylformamide at 0° C. 10 minutes after, 2.64 ml (27.0 mmol) of propyl iodide was gently added to the mixture. The mixture was stirred at room temperature for 2 hours and a half. After 150 ml of saturated ammonium chloride aqueous solution was added to the reaction solution, the mixture was extracted 3 times with chloroform. The extracts were combined and washed twice with a saturated aqueous sodium chloride. After drying over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure. 50% ether/n-hexane was added to the residue. The precipitates were taken out by filtration to give 2.09 g (yield, 84%) of Compound o as a light yellow powder.

1. extractionthe mixture was extracted 3 times with chloroform
2. washwashed twice with a saturated aqueous sodium chloride
3. dry with materialAfter drying over anhydrous sodium sulfate
4. customthe solvent was evaporated under reduced pressure
5. addition50% ether/n-hexane was added to the residue
6. filtrationThe precipitates were taken out by filtration
7. customto give