反应详情

To a solution of 2-[5-(2,6-diethyl-phenyl)-1-(4-isopropyl-phenyl)-1H-pyrrolo[2,3-c]pyridin-3-ylmethyl]-2-ethyl-butyric acid ethyl ester (100 mg, 0.19 mmol) in DCM (10 mL) at −78° C., DIBAL (1M solution in toluene, 0.95 mL, 0.9 mmol) is added and the mixture is allowed to gradually warm up room temperature, at which stirring is continued for 2 h. To the mixture, a saturated aqueous Rochelle's salt solution (10 mL) is added and stirring is continued for 1 h. The organic layer is separated and the aqueous is extracted with DCM. The combined organic extracts are washed with brine, dried (Na2SO4), and concentrated under reduced pressure. The residue is purified by chromatography on silica gel (Hexane/EtOAc, 2:1) to afford 2-[5-(2,6-diethyl-phenyl)-1-(4-isopropyl-phenyl)-1H-pyrrolo[2,3-c]pyridin-3-ylmethyl]-2-ethyl-butan-1-ol as colorless oil: LCMS m/z 483.21 (2.64 min)

1. stirringstirring
2. waitis continued for 1 h
3. customThe organic layer is separated
4. extractionthe aqueous is extracted with DCM
5. washThe combined organic extracts are washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated under reduced pressure
8. customThe residue is purified by chromatography on silica gel (Hexane/EtOAc, 2:1)