反应详情

The title compound of step 1 (0.88 g, 2.94 mmol) was dissolved in THF (35 mL) and mixed in drops with 2M phenylmagnesium chloride solution (5.1 mL, 10.2 mmol) with ice cooling. The reaction solution was heated to boiling for 8 h. For work up the solution was mixed with 20% NH4Cl solution (0.6 mL) and water (0.4 mL) with ice cooling, extracted with ether (3×25 mL), the ether solution was washed with water, dried (Na2SO4) and concentrated to low volume in a vacuum. The residue was purified by column chromatography with EtOH/EE (1:20). 2 fractions were obtained, wherein according to LCMS, inter alia, the more polar fraction (300 mg) contained the desired substance.

1. temperatureThe reaction solution was heated
2. extractionextracted with ether (3×25 mL)
3. washthe ether solution was washed with water
4. dry with materialdried (Na2SO4)
5. concentrationconcentrated to low volume in a vacuum
6. customThe residue was purified by column chromatography with EtOH/EE (1:20)
7. custom2 fractions were obtained