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Iodine → 2-Amino-5-chloro-3-iodopyridine

HRID 58651
Notes
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Reaction equation

HRID 58651 reaction equation
[I:1]I.[Cl:3][C:4]1[CH:5]=[CH:6][C:7]([NH2:10])=[N:8][CH:9]=1>C(O)C.S([O-])([O-])(=O)=O.[Ag+2]>[Cl:3][C:4]1[CH:5]=[C:6]([I:1])[C:7]([NH2:10])=[N:8][CH:9]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 2

HCID 807IodineHCID 661742-Amino-5-chloropyridine

Product 1

HCID 110760102-Amino-5-chloro-3-iodopyridineYield 64%

Reagents, catalysts & solvents 2

HCID 178418844HCID 178418844, compoundCatalystHCID 702EthanolSolvent

Procedure

Iodine (7.55 g; 29.73 mmol) was added to a mixture of 5-chloropyridin-2-amine (3.00 g; 22.87 mmol) and silver sulphate (9.36 g; 29.73 mmol) in ethanol (150 mL) and the mixture was stirred overnight at room temperature. The mixture was filtered over celite, washed with ethanol, and the filtrate concentrated under reduced pressure. The residue was dissolved in dichloromethane, and the solution was washed with a saturated aqueous solution of sodium thiosulphate. The organic layer was dried over magnesium sulphate, concentrated under reduced pressure and the crude material purified by flash chromatography on silica gel (eluent: 0 to 30% of ethyl acetate in heptane) to give 3.71 g (64%) of 5-chloro-3-iodopyridin-2-amine as a beige solid.

Workup

  1. filtrationThe mixture was filtered over celite
  2. washwashed with ethanol
  3. concentrationthe filtrate concentrated under reduced pressure
  4. dissolutionThe residue was dissolved in dichloromethane
  5. washthe solution was washed with a saturated aqueous solution of sodium thiosulphate
  6. dry with materialThe organic layer was dried over magnesium sulphate
  7. concentrationconcentrated under reduced pressure
  8. customthe crude material purified by flash chromatography on silica gel (eluent: 0 to 30% of ethyl acetate in heptane)

Sources & evidence

ORD record
ord-601e897bc3144f69904f9d03319b7ee7
Source dataset
uspto-grants-2016_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09434722B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes