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Aluminum(III) Chloride → 4-Amino-6-chloropyridin-2(1H)-one

HRID 2407807
Notes
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Reaction equation

HRID 2407807 reaction equation
[Cl:1][C:2]1[CH:7]=[C:6]([NH2:8])[CH:5]=[C:4]([O:9]CC)[N:3]=1.[Cl-].[Cl-].[Cl-].[Al+3]>C1(C)C=CC=CC=1>[NH2:8][C:6]1[CH:7]=[C:2]([Cl:1])[NH:3][C:4](=[O:9])[CH:5]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 6451240Aluminum(III) ChlorideHCID 534852242-Chloro-6-ethoxypyridin-4-amine

Product 1

HCID 585042194-Amino-6-chloropyridin-2(1H)-one

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

2-Chloro-6-ethoxypyridin-4-amine (10.0 g, prepared according to the reported preparation in J. Med. Chem., (2006), 49 (12), 3563-3580) and aluminum trichloride (19.3 g) were suspended in toluene (300 mL) and heated at reflux under a nitrogen atmosphere. The reaction mixture was cooled to room temperature and partitioned between saturated aqueous Rochelle's salt and ethyl acetate and vigorously stirred overnight. The biphasic mixture was filtered. The aqueous was repeatedly extracted with ethyl acetate. The combined organics were dried, magnesium sulfate and concentrated under reduced pressure to furnish the title compound (4.23 g), which was used without further purification, possessing the following physical data.

Workup

  1. customaccording to the reported preparation in J
  2. temperatureheated
  3. temperatureat reflux under a nitrogen atmosphere
  4. custompartitioned between saturated aqueous Rochelle's salt and ethyl acetate and vigorously stirred overnight
  5. filtrationThe biphasic mixture was filtered
  6. extractionThe aqueous was repeatedly extracted with ethyl acetate
  7. customThe combined organics were dried
  8. concentrationmagnesium sulfate and concentrated under reduced pressure

Sources & evidence

ORD record
ord-03b3171d315e40a0abfea0d6cd2f73d6
Source dataset
uspto-grants-2014_08
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08809538B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes