反应详情

温度

150 °C

A mixture of 4-chloro-2-(1-(5-methyl-6-(2,2,2-trifluoroethoxy)pyridin-3-yl)ethyl)-2,3-dihydro-1H-pyrrolo[3,4-c]pyridin-1-one (200 mg, 0.52 mmol, Intermediate-2, single enantiomer), zinc cyanide (300 mg, 1.56 mmol), and 1,1′-bis(diphenylphosphino)ferrocene-palladium(II)dichloride dichloromethane complex (42 mg, 0.052 mmol) in DMF (5 mL) is heated at 150° C. for 30 min by microwave irradiation. The mixture is filtered through a pad of Celite™. The Celite™ pad is washed with water, and EtOAc. The filtrate is washed with water, dried over sodium sulfate and concentrated under reduced pressure. The residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (3:1) to give 160 mg (80% yield) of the title compound as colorless oil.

1. filtrationThe mixture is filtered through a pad of Celite™
2. washThe Celite™ pad is washed with water, and EtOAc
3. washThe filtrate is washed with water
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (3:1)