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

HRID 1017795노트

반응식

HRID 1017795 반응식
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]

참가 물질

8

반응물 4

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

생성물 1

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

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-31f9fcdb7d0f4fb996b038725fc7271d
출처 데이터셋
uspto-grants-2002_11
특허 번호
US06479524B1

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