反应详情

2M phenylmagnesium chloride solution in THF (3.5 mL, 7.0 mmol) was slowly added in drops to a solution of the title compound of step 7 (1.00 g, 3.5 mmol) in abs. THF (10 mL) in a nitrogen atmosphere and with ice cooling at 10° C. The solution was stirred for 20 h at RT. Then 20% NH4Cl solution (5 mL) and water (2 mL) were added and the solution was extracted with ether (3×5 mL). The combined organic phases were washed with water (2 mL) and saturated NaCl solution (2 mL), dried over Na2SO4 and concentrated to low volume in a vacuum. By flash chromatography of the residue with chloroform/methanol (20:1) a salt of the product was obtained that was released with 1N NaOH, extracted with chloroform, dried over Na2SO4, and the solvent removed from it in a vacuum.

1. customat 10° C
2. extractionthe solution was extracted with ether (3×5 mL)
3. washThe combined organic phases were washed with water (2 mL) and saturated NaCl solution (2 mL)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated to low volume in a vacuum
6. customBy flash chromatography of the residue with chloroform/methanol (20:1) a salt of the product was obtained
7. extractionextracted with chloroform
8. dry with materialdried over Na2SO4
9. customthe solvent removed from it in a vacuum