Iodine → 2-Iodo-4-methyl-6-nitroaniline

HRID 1802806ノート

反応式

HRID 1802806 の反応式
[CH3:1][C:2]1[CH:8]=[CH:7][C:5]([NH2:6])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.[I:12]I>C(O)C.[N+]([O-])([O-])=O.[Ag+]>[I:12][C:7]1[CH:8]=[C:2]([CH3:1])[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5]=1[NH2:6]

参加物

5

反応物 2

HCID 807IodineHCID 69784-Methyl-2-nitroaniline

生成物 1

HCID 197351992-Iodo-4-methyl-6-nitroaniline収率 79.3%

試薬・触媒・溶媒 2

HCID 24470Silver Nitrate触媒HCID 702Ethanol溶媒

実験手順

4-Methyl-2-nitroaniline (20 g, 131.5 mmol) was dissolved in ethanol (300 ml), silver nitrate (27 g, 157.7 mmol) and iodine (40 g, 157.7 mmol) were added, and the mixture was stirred for 8 h at room temperature. After completion of the reaction, the reaction mixture was filtered through celite, washed with ethyl acetate (100 ml) and concentrated. Water was added, and the mixture was extracted with ethyl acetate, washed with saturated sodium chloride solution and dried over anhydrous magnesium sulfate to give 2-iodo-4-methyl-6-nitro-phenylamine (29 g, Yield 69%).

後処理

  1. customAfter completion of the reaction
  2. filtrationthe reaction mixture was filtered through celite
  3. washwashed with ethyl acetate (100 ml)
  4. concentrationconcentrated
  5. additionWater was added
  6. extractionthe mixture was extracted with ethyl acetate
  7. washwashed with saturated sodium chloride solution
  8. dry with materialdried over anhydrous magnesium sulfate

出典と根拠

ORDレコード
ord-0373e998c43a4518ae40c16048aa385b
出典データセット
uspto-grants-2013_01
特許番号
US08349885B2

反応ノート

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