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[(4-Methoxy-2-nitrophenyl)imino]ethyl acetate → 7-Methoxy-3,4-dihydroquinoxalin-2(1H)-one

HRID 1847079
Notes
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Reaction equation

HRID 1847079 reaction equation
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]=[CH:10][CH2:11][O:12]C(=O)C)=[C:5]([N+:16]([O-])=O)[CH:4]=1>CO.[Pd].ClCCl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:6]([NH:9][CH2:10][C:11](=[O:12])[NH:16]2)=[CH:7][CH:8]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 1

HCID 86725002[(4-Methoxy-2-nitrophenyl)imino]ethyl acetate

Product 1

HCID 6012927-Methoxy-3,4-dihydroquinoxalin-2(1H)-one

Reagents, catalysts & solvents 3

HCID 23938PalladiumCatalystHCID 887MethanolSolventHCID 6344DichloromethaneSolvent

Procedure

The obtained [(4-methoxy-2-nitrophenyl)imino]ethyl-acetate crude product was dissolved in methanol (30 ml) and 10% palladium on carbon (50% wet, 1.20 g) was added thereto and the mixture was stirred at room temperature for 3 hours under a hydrogen gas atmosphere. The catalyst was removed by filtration using celite and the filtrate was concentrated under reduced pressure to yield 1.733 g of a crude product of 7-methoxy-3,4-dihydroquinoxalin-2(1H)-one. In dichloromethane (12 ml) was dissolved 518 mg of the obtained crude product of 7-methoxy-3,4-dihydroquinoxalin-2(1H)-one, and under a nitrogen gas atmosphere in an ice bath, N,N-diisopropylethylamine (0.604 ml, 3.47 mmol) and subsequently benzyl chloroformate (0.408 ml, 2.77 mmol) were added thereto. Then, the mixture was stirred at room temperature for 17 hours, a saturated sodium hydrogen carbonate aqueous solution was added thereto and the resultant was extracted with dichloromethane. The extract was combined, dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to yield 291 mg (40%) of the title compound in the form of a light red solid.

Workup

  1. customThe catalyst was removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. customto yield 1.733 g of a crude product of 7-methoxy-3,4-dihydroquinoxalin-2(1H)-one

Sources & evidence

ORD record
ord-7d16e9724fef4323a7a7203f343e6142
Source dataset
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08952010B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes