[F:1][C:2]1[C:10]([F:11])=[CH:9][C:8](O)=[CH:7][C:3]=1C(O)=O.[C:13]([O-:16])([O-])=[O:14].[K+].[K+].[CH3:19]I.CN([CH:24]=[O:25])C>CCOC(C)=O>[CH3:19][O:16][C:13](=[O:14])[C:9]1[CH:8]=[C:7]([O:25][CH3:24])[CH:3]=[C:2]([F:1])[C:10]=1[F:11]To a solution of 2,3-difluoro-5-hydroxy-benzoic acid [749230-51-1] (1.00 g, 5.74 mmol; Melford Laboratories Ltd) in DMF (20 mL) was added K2CO3 (1.99 g, 14.4 mmol) and MeI (0.79 mL, 12.6 mmol), followed by stirring at RT overnight. The reaction mixture was diluted with EtOAc, the organics were washed with a saturated aqueous NH4Cl solution (50 mL) and a saturated aqueous NaHCO3 solution, dried (Phase separator) and evaporated under reduced pressure. The residue was purified by flash column chromatography on silica gel (c-hexane/EtOAc 3:1) to afford the title compound as a colorless oil. TLC, Rf (c-hexane/EtOAc 3:1)=0.37; MS (LC/MS): 203.0 [M+H]+; tR (HPLC conditions c): 4.72 min.
Wird geladen…
