2,5-Dimethylaniline → (4-Iodo-2,5-Dimethylphenyl)Amine

HRID 1017795ノート

反応式

HRID 1017795 の反応式
I(Cl)(=O)=O.[I:5](Cl)(=O)=O.C([N+](C)(C)C)C1C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+].[CH3:26][C:27]1[CH:33]=[CH:32][C:31]([CH3:34])=[CH:30][C:28]=1[NH2:29].S(S([O-])=O)([O-])(=O)=O.[Na+].[Na+]>CO.ClCCl.O>[CH3:26][C:27]1[CH:33]=[C:32]([I:5])[C:31]([CH3:34])=[CH:30][C:28]=1[NH2:29]

参加物

8

反応物 4

HCID 72592,5-DimethylanilineHCID 11430Potassium CarbonateHCID 656671Sodium PyrosulfiteHCID 56924451Trimethylbenzylammonium Dichloroiodate

生成物 1

HCID 4770984(4-Iodo-2,5-Dimethylphenyl)Amine

試薬・触媒・溶媒 3

HCID 887Methanol溶媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

25.0 g (71.8 mmol) of benzyltrimethylammonium dichloriodate and 12.8 g (92.5 mmol) of potassium carbonate are added to a solution of 8.8 ml of (70.8 mmol) of 2,5-dimethylaniline in 250 ml of methanol and 600 ml of dichloromethane and stirred for 1 hour at ambient temperature. Then the inorganic salts are suction filtered and the solvent is distilled off. The residue is combined with a solution of 13.5 g (70.8 mmol) of sodium pyrosulphite in 640 ml of water and extracted with ether. The combined organic extracts are dried over sodium sulphate and evaporated down. The crude product is triturated with petroleum ether, suction filtered and dried.

後処理

  1. filtrationfiltered
  2. distillationthe solvent is distilled off
  3. extractionextracted with ether
  4. dry with materialThe combined organic extracts are dried over sodium sulphate
  5. customevaporated down
  6. customThe crude product is triturated with petroleum ether, suction
  7. filtrationfiltered
  8. customdried

出典と根拠

ORDレコード
ord-31f9fcdb7d0f4fb996b038725fc7271d
出典データセット
uspto-grants-2002_11
特許番号
US06479524B1

反応ノート

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