Methanol → Methyl 2-bromo-3-fluorobenzoate

To a suspension of 2-bromo-3-fluorobenzoic acid (300 mg, 1.37 mmol) in methanol (10 mL) at rt, was added SOCl2 (0.11 mL, 1.51 mmol) and the mixture was stirred at rt for 18 h. The solvent was distilled off under reduced pressure. The crude was basified by adding saturated aqueous NaHCO3 solution and the aqueous layer was extracted with EtOAc (3×25 mL). The combined organic layers were dried over Na2SO4, filtered and concentrated. The obtained crude product was used in the next step without further purification.

1. distillationThe solvent was distilled off under reduced pressure
2. additionby adding saturated aqueous NaHCO3 solution
3. extractionthe aqueous layer was extracted with EtOAc (3×25 mL)
4. dry with materialThe combined organic layers were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe obtained crude product
8. customwas used in the next step without further purification

ORDレコード

ord-d2262f51bbf44f65a231c0dc5480626b

出典データセット

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09388191B2