C1N=CN(C(N2C=NC=C2)=O)C=1.C1COCC1.[Br:18][C:19]1[CH:27]=[C:26]([F:28])[C:25]([F:29])=[CH:24][C:20]=1[C:21](O)=[O:22].[BH4-].[Na+]>CCOC(C)=O.C([O-])(O)=O.[Na+].O>[Br:18][C:19]1[CH:27]=[C:26]([F:28])[C:25]([F:29])=[CH:24][C:20]=1[CH2:21][OH:22]Solid CDI (4.3 g, 26.4 mmol) was added to a THF solution (130 mL) of 2-bromo-4,5-difluorobenzoic acid and the solution was refluxed. After 3 h the resulting mixture was cooled to room temperature and a water solution (26 mL) of NaBH4 (666 mg, 17.6 mmol) was added. After 10 min the resulting mixture was diluted with EtOAc and 10% aqueous NaHCO3 and the layers were separated. The organic layer was washed with water and brine, dried (Na2SO4), concentrated, and purified via column chromatography to yield the title compound.
Wird geladen…
