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

HRID 59799

反応式

HRID 59799 の反応式
[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]

参加物

4

反応物 2

HCID 807IodineHCID 73194-Methyl-3-nitrobenzoic acid

生成物 1

HCID 596277773-Iodo-4-methyl-5-nitrobenzoic acid収率 95%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
85 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6ddb5c05d6114e6ebc338e4750958068
出典データセット
uspto-grants-2016_09
特許番号
US09440956B2

関連ノート

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