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

HRID 367012노트

반응식

HRID 367012 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9bb366711f7b4f87b41193cf93bbfc82
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06133260

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