Methanol → Benzoic acid, 2-bromo-5-fluoro-, methyl ester

To a solution of 2-bromo-5-fluorobenzoic acid (9) (21.90 g, 100 mmol) in methanol (100 mL) was added conc. H2SO4 (2 mL). The mixture was heated at reflux for 21 h. Most of the solvent was evaporated and diluted with water (200 mL). The mixture was extracted with EtOAc (150 mL×2). The combined extracts were washed with saturated NaHCO3 and brine, dried over MgSO4, and concentrated to give methyl 2-bromo-5-fluorobenzoate (10).

1. temperatureThe mixture was heated
2. temperatureat reflux for 21 h
3. customMost of the solvent was evaporated
4. additiondiluted with water (200 mL)
5. extractionThe mixture was extracted with EtOAc (150 mL×2)
6. washThe combined extracts were washed with saturated NaHCO3 and brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated

ORD-Eintrag

ord-c0f3a646246d4f00b001da8558ac0502

Quelldatensatz

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09340523B2