反应详情

Under nitrogen atmospher, To a solution of 178 mg of compound obtained in Step 7-2-1 in DMF (1.8 ml) was added 170 mg sodium bis-(trimethylsilyl) amide (38% THF solution) under ice cooling, and the reaction mixture was stirred for 15 minutes at the same temperature. Thereafter a solution of 178 mg of compound obtained in Step 7-2-3 in THF (500 μL) was added, and the solution was stirred at the same temperature for one hour, and at room temperature for 15 hours. To the reaction solution was added EtOAc and an aqueous solution of 5% K2CO3, and was stirred for 10 minutes. Liquid separation was performed, and the aqueous layer was extracted with EtOAc. The combined organic layer was washed in water and saturated brine, dried over MgSO4, then, the drying agent was separated by filtration, and the solvent was evaporated under reduced pressure. The obtained residue was subjected to column chromatography (silicagel 60; mobile phase: EtOAc/n-hexane=1/1; v/v) to obtain a brown oil (8 mg). Among the obtained brown oil, 2.0 mg was purified by thin layer chromatography (silicagel 60F254; 1 mm thick; mobile phase: EtOAc/n-hexane=7/3; v/v) to obtain 0.13 mg of the title compound (yellow oil).

1. stirringthe solution was stirred at the same temperature for one hour
2. waitat room temperature for 15 hours
3. customLiquid separation
4. extractionthe aqueous layer was extracted with EtOAc
5. washThe combined organic layer was washed in water
6. dry with materialsaturated brine, dried over MgSO4
7. customthe drying agent was separated by filtration
8. customthe solvent was evaporated under reduced pressure