Methanol → Methyl 4-bromobenzoate

HRID 36028

반응식

HRID 36028 반응식
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[CH:4][CH:3]=1.S(=O)(=O)(O)O.[CH3:16]O>>[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH3:16])=[O:7])=[CH:4][CH:3]=1

참가 물질

4

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 114644-Bromobenzoic acid

생성물 1

HCID 12081Methyl 4-bromobenzoate수율 87.5%

실험 절차

4-Bromobenzoic acid (9.98 kg, 48 mol) was suspended in 40 kg of methanol. Sulfuric acid (2 kg, 20 mol) was added and the mixture was heated under reflux for approximately 5 hours. The mixture was cooled over 10 hours to -10° C. and allowed to stand for 5 hours giving a crystalline product. The product was isolated by filtration and the filter cake was washed with methanol (2×3 L). Drying gave methyl 4-bromobenzoate (9.97 kg, 42 mol), m.p. 78°-78.7° C.

후처리

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for approximately 5 hours
  3. temperatureThe mixture was cooled over 10 hours to -10° C.
  4. customgiving a crystalline product
  5. customThe product was isolated by filtration
  6. washthe filter cake was washed with methanol (2×3 L)
  7. customDrying

출처 및 근거

ORD 기록
ord-bd225c2486bf4e2c8393dcbbeb4f722c
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05412102

연결된 노트

불러오는 중…