Hydrochloric Acid → 4-Bromo-2-fluoro-5-methylbenzoic acid

NaH2PO4 (418 mg, 3.48 mmol) in H2O (17.6 ml), a 35% aqueous H2O2 solution (2.5 ml, 25.7 mmol) and NaClO2 (2.23 g, 24.7 mmol) in H2O (34.9 ml) were sequentially added to a mixture of 4-bromo-2-fluoro-5-methyl-benzaldehyde (3.74 g, 17.2 mmol) in MeCN (52 ml) at 0° C. The mixture was stirred at room temperature for 14 hours, and then made acidic (pH 3) with a 10% aqueous HCl solution and extracted with ethyl acetate (3×100 ml). The organic layers were washed with H2O (70 ml), and then dried over MgSO4 and concentrated under reduced pressure to give 4-bromo-2-fluoro-5-methyl-benzoic acid as a pale orange solid (4.02 g, 100%).

1. extractionextracted with ethyl acetate (3×100 ml)
2. washThe organic layers were washed with H2O (70 ml)
3. dry with materialdried over MgSO4
4. concentrationconcentrated under reduced pressure

ORDレコード

ord-82da6db446af4e3b96f1cd47575b001d

出典データセット

uspto-grants-2015_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09169254B2