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

HRID 524106

反応式

HRID 524106 の反応式
[Br:1][C:2]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].OS(O)(=O)=O.[CH3:17]O>>[Br:1][C:2]1[CH:10]=[CH:9][C:8]([F:11])=[CH:7][C:3]=1[C:4]([O:6][CH3:17])=[O:5]

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 27781812-Bromo-5-fluorobenzoic acid

生成物 1

HCID 138875Benzoic acid, 2-bromo-5-fluoro-, methyl ester

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c0f3a646246d4f00b001da8558ac0502
出典データセット
uspto-grants-2016_05
特許番号
US09340523B2

関連ノート

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