Methanol → Methyl 3-bromobenzoate

HRID 54195

반응식

HRID 54195 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].[CH3:11]O>S(=O)(=O)(O)O>[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([O:7][CH3:11])=[O:6]

참가 물질

4

반응물 2

HCID 887MethanolHCID 114563-Bromobenzoic acid

생성물 1

HCID 12070Methyl 3-bromobenzoate수율 85%

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

실험 절차

Part A: 3-Bromobenzoic acid (1.1 g, 5.47 mmol) was dissolved in methanol (20 ml) in a 50 ml flask. Concentrated sulfuric acid (2 drops) was added and the mixture was refluxed under nitrogen for ten hours then concentrated under reduced pressure. The residue was mixed with dichloromethane (20 ml) and saturated sodium bicarbonate solution (10 ml). The organic material was separated, dried (MgSO4) and concentrated under reduced pressure. The residue was flushed through silica gel with hexane/ethyl acetate (3:1), and concentrated which provided methyl 3-bromobenzoate (1.0 g, 85%).

후처리

  1. temperaturethe mixture was refluxed under nitrogen for ten hours
  2. concentrationthen concentrated under reduced pressure
  3. additionThe residue was mixed with dichloromethane (20 ml) and saturated sodium bicarbonate solution (10 ml)
  4. customThe organic material was separated
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was flushed through silica gel with hexane/ethyl acetate (3:1)
  8. concentrationconcentrated which

출처 및 근거

ORD 기록
ord-02beae4f681d488aae48056e2215c553
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05622937

연결된 노트

불러오는 중…