Iodine → 3-Iodo-4-methyl-5-nitrobenzoic acid

HRID 446220

반응식

HRID 446220 반응식
[I:1]I.[CH3:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][C:5]=1[N+:13]([O-:15])=[O:14]>S(=O)(=O)(O)O>[I:1][C:12]1[CH:11]=[C:7]([CH:6]=[C:5]([N+:13]([O-:15])=[O:14])[C:4]=1[CH3:3])[C:8]([OH:10])=[O:9]

참가 물질

4

반응물 2

HCID 807IodineHCID 73194-Methyl-3-nitrobenzoic acid

생성물 1

HCID 596277773-Iodo-4-methyl-5-nitrobenzoic acid수율 95%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
85 °C

실험 절차

To a mixture of iodine (19.6 g, 77.3 mmol) in fuming sulfuric acid (35 mL) was added 4-methyl-3-nitro-benzoic acid (10.0 g, 55.2 mmol). The mixture was stirred at 85° C. over night, then cooled to room temperature and poured over ice. The mixture was partitioned between ethyl acetate and aqueous sodium bisulfite, and the organic layer was separated, dried over MgSO4, filtered and concentrated under reduced pressure to give 16.06 g (95%) of 3-iodo-4-methyl-5-nitro-benzoic acid.

후처리

  1. temperaturecooled to room temperature
  2. additionpoured over ice
  3. customThe mixture was partitioned between ethyl acetate and aqueous sodium bisulfite
  4. customthe organic layer was separated
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-0b8f3e28eb3d4330a914fec7f029f573
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08476457B2

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