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

HRID 59799

반응식

HRID 59799 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, filterd 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, filterd
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-6ddb5c05d6114e6ebc338e4750958068
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440956B2

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