反应详情

温度

100 °C

A mixture of 4-chloro-2-(1-(5-chloro-6-(2,2,2-trifluoroethoxy)pyridin-3-yl)ethyl)-2,3-dihydro-1H-pyrrolo[3,4-c]pyridin-1-one (200 mg, 0.49 mmol, Intermediate-9, single enantiomer), palladium(II) acetate (33 mg, 0.15 mmol, 1,3-bis(diphenylphosphino)propane (20 mg, 0.049 mmol), and triethylamine (150 mg, 1.5 mmol) in DMF/EtOH (2:1, 14 mL) is heated at 100° C. overnight under carbon monoxide atmosphere. The mixture is diluted with water, and filtered through a pad of Celite™. The Celite™ pad is washed with EtOAc/toluene (2:1) mixed solvent. The filtrate is washed with water, brine, and dried over sodium sulfate. The organic layer is filtered, and the filtrate is concentrated. The residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (1:1 to 1:2) to give 160 mg (73% yield) of the title compound as yellow solid.

1. filtrationfiltered through a pad of Celite™
2. washThe Celite™ pad is washed with EtOAc/toluene (2:1)
3. additionmixed solvent
4. washThe filtrate is washed with water, brine
5. dry with materialdried over sodium sulfate
6. filtrationThe organic layer is filtered
7. concentrationthe filtrate is concentrated
8. customThe residue is purified by column chromatography on silica gel eluting with n-hexane/EtOAc (1:1 to 1:2)