Methanol → Methyl 2-chloro-5-fluorobenzoate

HRID 524118ノート

反応式

HRID 524118 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-4b903d616e1e43ed9e2a281491046620
出典データセット
uspto-grants-2016_05
特許番号
US09340523B2

反応ノート

読み込み中…