反应详情

In 2.2 ml of DMF was dissolved 335 mg (0.61 mmol) of Compound 47 obtained in Example 47, 25 mg (0.61 mmol) of 60% sodium hydride was added at ice-cooling, and stirred at ice-cooling for 20 minutes. 0.042 ml (0.67 mmol) of methyl iodide was added to the above reaction mixture and stirred at room tempareture for 2 hours. Saturated ammonium chloride solution was added and resulting precipitate was collected by filtration, washed with water, dried at heating, purified by silica gel column chromatography (eluent: chloroform/methanol=100/1) and recrystallized from ethanol/ether to give 168 mg (yield: 49%) of Compound 48 as white crystals.

1. additionwas added at ice-
2. temperaturecooling
3. temperaturecooling for 20 minutes
4. stirringstirred at room tempareture for 2 hours
5. customresulting precipitate
6. filtrationwas collected by filtration
7. washwashed with water
8. customdried
9. temperatureat heating
10. custompurified by silica gel column chromatography (eluent: chloroform/methanol=100/1)
11. customrecrystallized from ethanol/ether