反应详情

To a solution of NaH (0.62 g, 15.5 mmol, 60% NaH) in 40 mL of DMF, 5-methanesulfonyl-2,3-dihydro-1H-indole (1.9 g, 9.63 mmol) was added and the mixture was stirred at room temperature for 30 minutes. 17a (3.09 g, 9.88 mmol) was added in DMF and the mixture was heated at 85° C. for 17 h. After cooling to room temperature, brine was added (200 mL) and the mixture was extracted with DCM (200 mL then 3×500 mL). The combined extracts were washed with brine (3×100 mL), dried, filtered and evaporated. The residue was purified by flash chromatography (eluent: 25 to 100% EtOAc in hexane with 0.1% triethylamine) to afford 2.83 g (62%) of 17b.

1. temperaturethe mixture was heated at 85° C. for 17 h
2. temperatureAfter cooling to room temperature
3. extractionthe mixture was extracted with DCM (200 mL
4. washThe combined extracts were washed with brine (3×100 mL)
5. customdried
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified by flash chromatography (eluent: 25 to 100% EtOAc in hexane with 0.1% triethylamine)