反応 #595373

ord-5070471ea1764e26830308311c49e807

反応方程式

O=C(O)c1cc(F)c(Br)cc1F
4-bromo-2,5-difluorobenzoic acid
CO
methanol
COC(=O)c1cc(F)c(Br)cc1F
title compound
COC(=O)c1cc(F)c(Br)cc1F
methyl 4-bromo-2,5-difluorobenzoate

反応条件

温度
65°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The mixture was concentrated
  2. 2
    workup.ADDITIONThen MeOH was added
  3. 3
    濃縮the mixture was concentrated again
  4. 4
    その他The residue was purified by flash chromatography (Pentane/EtOAc=4:1)

実験手順

A mixture of 4-bromo-2,5-difluorobenzoic acid (i-7b) (0.48 g, 2 mmol) and methanol (10 mL, saturated with gaseous HCl) was heated at 65° C. for 2 h. The mixture was concentrated. Then MeOH was added and the mixture was concentrated again. The residue was purified by flash chromatography (Pentane/EtOAc=4:1) to give the title compound. LCMS (ESI) calc'd for C8H5BrF2O2 [M+H]+: 251. found: 251.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09095583B2uspto-grants-2015_08