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

HRID 430590ノート

反応式

HRID 430590 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-benzoyl fluoride are added dropwise to 1460 ml of methanol and 340 g of triethylamin, while cooling with ice. The mixture is stirred at room temperature for 1 hour. The reaction mixture is concentrated in vacuo and the resulting residue is taken up in water and methylene chloride. The water is extracted with methylene chloride once more. The organic phase is dried with Na2CO3 and concentrated in vacuo. The resulting residue is distilled in vacuo.

後処理

  1. temperaturewhile cooling with ice
  2. concentrationThe reaction mixture is concentrated in vacuo
  3. extractionThe water is extracted with methylene chloride once more
  4. dry with materialThe organic phase is dried with Na2CO3
  5. concentrationconcentrated in vacuo
  6. distillationThe resulting residue is distilled in vacuo

出典と根拠

ORDレコード
ord-105e54b9e56840beb2bb29144385b04e
出典データセット
uspto-grants-2001_11
特許番号
US06323213B1

反応ノート

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