Methanol → Methyl 3-bromo-2,4,5-trifluorobenzoate

HRID 367012ノート

反応式

HRID 367012 の反応式
[Br:1][C:2]1[C:3]([F:13])=[C:4]([CH:8]=[C:9]([F:12])[C:10]=1[F:11])[C:5](F)=[O:6].[CH3:14][OH:15]>C(N(CC)CC)C>[Br:1][C:2]1[C:3]([F:13])=[C:4]([CH:8]=[C:9]([F:12])[C:10]=1[F:11])[C:5]([O:15][CH3:14])=[O:6]

参加物

4

反応物 2

HCID 887MethanolHCID 141498723-Bromo-2,4,5-trifluorobenzoyl fluoride

生成物 1

HCID 18459836Methyl 3-bromo-2,4,5-trifluorobenzoate

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

772 g of 3-bromo-2,4,5-trifluoro-benzoylfluoride are added dropwise with ice-cooling to a mixture of 1460 ml of methanol and 340 g of triethylamine. Stirring is carried out at room temperature for 1 hour. The reaction mixture is concentrated, the residue is taken up in water and methylene chloride, and the aqueous phase is again extracted by shaking with methylene chloride. After drying the organic phase over sodium sulphate, it is concentrated and the residue is distilled in vacuo. 752.4 g of methyl 3-bromo-2,4,5-trifluoro-benzoate of boiling point 122° C./20 mbar are obtained.

後処理

  1. concentrationThe reaction mixture is concentrated
  2. extractionmethylene chloride, and the aqueous phase is again extracted
  3. stirringby shaking with methylene chloride
  4. dry with materialAfter drying the organic phase over sodium sulphate, it
  5. concentrationis concentrated
  6. distillationthe residue is distilled in vacuo

出典と根拠

ORDレコード
ord-9bb366711f7b4f87b41193cf93bbfc82
出典データセット
uspto-grants-2000_10
特許番号
US06133260

反応ノート

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