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Chloroacetyl chloride → 5-methyl-1H-pyrido[2,3-b][1,4]oxazin-2-one

HRID 1943746
Notes
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Reaction equation

HRID 1943746 reaction equation
[NH2:1][C:2]1[C:3]([OH:9])=[N:4][CH:5]=[C:6](C)[CH:7]=1.Cl[CH2:11][C:12](Cl)=[O:13].[C:15](=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:15][N:4]1[CH:3]2[O:9][CH2:11][C:12](=[O:13])[NH:1][C:2]2=[CH:7][CH:6]=[CH:5]1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 3

HCID 6577Chloroacetyl chlorideHCID 11430Potassium CarbonateHCID 178430713HCID 178430713, compound

Product 1

HCID 669367555-methyl-1H-pyrido[2,3-b][1,4]oxazin-2-oneYield 24.1%

Reagents, catalysts & solvents 1

HCID 6228DimethylformamideSolvent

Procedure

3-amino-5-methyl-pyridin-2-ol (1.32 g, 10.6 mmol) was dissolved in 50 ml of anhydrous N,N-dimethyl formamide under nitrogen atmosphere, and chloroacetyl chloride solution (1.02 ml, 12.72 mmol) was added thereto dropwise at room temperature. After stirring for 30 minutes, potassium carbonate (3.7 g, 26.5 mmol) was added thereto dropwise at room temperature, and the reaction mixture was heated to 100□ and then stirred for 18 hours. The reaction mixture was cooled to room temperature and the reaction was quenched by adding water. The organic layer was extracted with ethyl acetate, and the combined organic layer was washed with water and saturated saline solution, dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure to obtain straw yellow solid (424 mg). The resulting solid was used in the next step without further purification.

Workup

  1. customdropwise at room temperature
  2. stirringstirred for 18 hours
  3. temperatureThe reaction mixture was cooled to room temperature
  4. customthe reaction was quenched
  5. additionby adding water
  6. extractionThe organic layer was extracted with ethyl acetate
  7. washthe combined organic layer was washed with water and saturated saline solution
  8. dry with materialdried over anhydrous sodium sulfate (Na2SO4)
  9. filtrationfiltered
  10. customevaporated under reduced pressure

Sources & evidence

ORD record
ord-07ce11b96d2c4160bfc8bc5afd657df0
Source dataset
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08394792B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes