Application of 33070-32-5, A common heterocyclic compound, 33070-32-5, name is 5-Bromo-2,2-difluorobenzodioxole, molecular formula is C7H3BrF2O2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
a) 2,2-Difluoro-5-(3-fluoro-4-nitrophenyl)-1 ,3-benzodioxoleA slurry of 5-bromo-2,2-difluoro-1 ,3-benzodioxole (1.23 g, 5.2 mmol), 4-N- BOC-amino-3-fluorophenylboronic acid (1.58 g, 6.2 mmol), [1,1′- bis(diphenylphosphino)ferrocene]dichloropalladium (II) dichloromethane adduct (0.131 g, 0.16mmol), and 2M aqueous sodium carbonate solution (7.8 mL, 15.6 mmol) in 1 ,4-dioxane (25.0 mL) was heated at reflux for 2.5 hours then cooled to ambient temperature. The reaction was dried over sodium sulfate then filtered and evaporated under reduced pressure to a residue. Purification by column chromatography on silica (0-65% gradient of ethyl acetate in hexanes) gave 1 ,1- dimethylethyl [4-(2,2-difluoro-1 ,3-benzodioxol-5-yl)-2-fluorophenyl]carbamate as a waxy white solid (54%).A solution of 1 ,1-dimethylethyl [4-(2,2-difluoro-1 ,3-benzodioxol-5-yl)-2- fluorophenyl]carbamate (0.992 g, 2.70 mmol) in 1 :1 trifluoroacetic acid and dichloromethane (20 mL) was stirred at ambient temperature for 1.5 hours then EPO
The synthetic route of 33070-32-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; SMITHKLINE BEECHAM CORPORATION; WO2006/113432; (2006); A2;,
Bromide – Wikipedia,
bromide – Wiktionary