[Br:1]Br.[CH3:3][O:4][C:5](=[O:14])[C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[C:8]([F:13])[CH:7]=1.C(OC)(=O)C.S([O-])([O-])=O.[Na+].[Na+].[Cl-].[Na+]>C(Cl)Cl.C(O)(=O)C.O>[CH3:3][O:4][C:5](=[O:14])[C:6]1[CH:7]=[C:8]([F:13])[C:9]([OH:12])=[C:10]([Br:1])[CH:11]=1During 30 min, 5.64 g (35.27 mmol) of bromine were added to a solution of 5.00 g (29.39 mmol) of 3-fluoro-4-hydroxy-benzoic acid methyl ester in 30 ml of DCM and 30 ml of acetic acid at 0° C. After stirring overnight, 200 ml of methyl acetate were added. The resulting solution was extracted with a solution of 7.56 g (60 mmol) of sodium sulfite in 50 ml of water, a saturated sodium chloride solution and water. The organic phase was dried over sodium sulfate, filtered and evaporated. The resulting white solid (7.2 g) was used in the next step without further purification.
読み込み中…
