反应详情

Compound 134 (10.7 g, 30.3 mmol) was dissolved in THF (240 ml), and a THF solution of 2.0 mol/L phenylmagnesium chloride (60.6 mL, 121 mmol) was added thereto at 0° C. in an atmosphere of argon, followed by stirring at room temperature for 2 hours. The reaction mixture was poured into a saturated aqueous solution of ammonium chloride, followed by extraction with ethyl acetate. The organic layer was washed with a saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and then the solvent was distilled away under reduced pressure. The resulting residue was purified through silica gel column chromatography (hexane:ethyl acetate=3:1) to afford the entitled Compound 135 (6.18 g, 55%).

1. customat 0° C.
2. extractionfollowed by extraction with ethyl acetate
3. washThe organic layer was washed with a saturated aqueous solution of sodium chloride
4. dry with materialdried over anhydrous magnesium sulfate
5. distillationthe solvent was distilled away under reduced pressure
6. customThe resulting residue was purified through silica gel column chromatography (hexane:ethyl acetate=3:1)