Methanol → Methyl 2-chloro-5-fluorobenzoate

HRID 240285ノート

反応式

HRID 240285 の反応式
[Cl: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>>[Cl: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 3028882-Chloro-5-fluorobenzoic acid

生成物 1

HCID 23331706Methyl 2-chloro-5-fluorobenzoate

実験手順

To a solution of 2-chloro-5-fluorobenzoic acid (22) (35.0 g, 200 mmol) in methanol (350 mL) was added cone. H2SO4 (5 mL). The mixture was heated at reflux for 24 h. Most of the solvent was evaporated, and the resulting mixture was diluted with water (300 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-chloro-5-fluorobenzoate (23).

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 24 h
  3. customMost of the solvent was evaporated
  4. additionthe resulting mixture was diluted with water (300 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-af7de7e4714440f796b4118a310ba488
出典データセット
uspto-grants-2014_02
特許番号
US08648073B2

反応ノート

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