Methanol → Benzoic acid, 2-bromo-5-fluoro-, methyl ester

HRID 524106

반응식

HRID 524106 반응식
[Br: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>>[Br: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]

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 27781812-Bromo-5-fluorobenzoic acid

생성물 1

HCID 138875Benzoic acid, 2-bromo-5-fluoro-, methyl ester

실험 절차

To a solution of 2-bromo-5-fluorobenzoic acid (9) (21.90 g, 100 mmol) in methanol (100 mL) was added conc. H2SO4 (2 mL). The mixture was heated at reflux for 21 h. Most of the solvent was evaporated and diluted with water (200 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-bromo-5-fluorobenzoate (10).

후처리

  1. temperatureThe mixture was heated
  2. temperatureat reflux for 21 h
  3. customMost of the solvent was evaporated
  4. additiondiluted with water (200 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

출처 및 근거

ORD 기록
ord-c0f3a646246d4f00b001da8558ac0502
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09340523B2

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