反应详情

To a RT solution of 4-chloro-1H-pyrrolo[2,3-b]pyridine (200 mg, 1.31 mmol) in DMF (5 mL) was added NaH (60% in mineral oil, 57.7 mg, 1.44 mmol) followed by methanesulfonic acid 3-chloro-1-phenyl-propyl ester (326 mg, 1.31 mmol). The reaction mixture was stirred at RT overnight, poured into ice-water, and extracted with EtOAc. The organic layer was washed with brine, dried over MgSO4, filtered and concentrated to yield 4-Chloro-1-(3-chloro-1-phenyl-propyl)-1H-pyrrolo[2,3-b]pyridine as a mixture with the cyclization product 8-Chloro-3-phenyl-4,5-dihydro-3H-2a-aza-5a-azonia-acenaphthylene. The mixture was used in the next step without purification.

1. extractionextracted with EtOAc
2. washThe organic layer was washed with brine
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated