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

HRID 1466474ノート

反応式

HRID 1466474 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.[I:12]I>C(O)C.[N+]([O-])([O-])=O.[Ag+]>[NH2:8][C:5]1[C:4]([N+:9]([O-:11])=[O:10])=[CH:3][C:2]([CH3:1])=[CH:7][C:6]=1[I:12]

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

Commercially available 4-methyl-2-nitro-phenylamine (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 thereto, and the mixture was stirred for 8 h at room temperature. After completion of the reaction, the reaction mixture was filtered through a cellite, washed with 100 mL of ethyl acetate, and concentrated. Water was added to the residue, which was then extracted with ethyl acetate, washed with saturated sodium chloride solution, and dried over anhydrous magnesium sulfate to give the title compound (29 g, Yield 69%).

後処理

  1. customAfter completion of the reaction
  2. filtrationthe reaction mixture was filtered through a cellite
  3. washwashed with 100 mL of ethyl acetate
  4. concentrationconcentrated
  5. additionWater was added to the residue, which
  6. extractionwas then 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-d64dc385be1249189cd881876e7fb1df
出典データセット
uspto-grants-2015_04
特許番号
US09000028B2

反応ノート

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