Methanol → Methyl 4-bromo-2,5-difluorobenzoate

HRID 508191

反応式

HRID 508191 の反応式
[Br:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([F:12])[CH:3]=1.[CH3:13]O>>[Br:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([O:8][CH3:13])=[O:7])=[C:4]([F:12])[CH:3]=1

参加物

3

反応物 2

HCID 887MethanolHCID 8228574-Bromo-2,5-difluorobenzoic acid

生成物 1

HCID 66887346Methyl 4-bromo-2,5-difluorobenzoate

反応条件

温度
65 °C

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.

後処理

  1. concentrationThe mixture was concentrated
  2. additionThen MeOH was added
  3. concentrationthe mixture was concentrated again
  4. customThe residue was purified by flash chromatography (Pentane/EtOAc=4:1)

出典と根拠

ORDレコード
ord-5070471ea1764e26830308311c49e807
出典データセット
uspto-grants-2015_08
特許番号
US09095583B2

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