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Aluminium lithium hydride → 7-Chloro-1-(3-hydroxypropyl)imidazo[1,5-a]quinoxalin-4(5H)-one

HRID 576830
Notes
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Reaction equation

HRID 576830 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[C:12]([CH2:15][CH2:16][C:17](OCC)=[O:18])=[N:13][CH:14]=[C:7]1[C:6](=[O:22])[NH:5]2.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]1[C:12]([CH2:15][CH2:16][CH2:17][OH:18])=[N:13][CH:14]=[C:7]1[C:6](=[O:22])[NH:5]2
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 21226445Aluminium lithium hydrideHCID 59198693Ethyl 3-(7-chloro-4-oxo-4,5-dihydroimidazo-[1,5-a]quinoxalin-1-yl)propanoate

Product 1

HCID 591985737-Chloro-1-(3-hydroxypropyl)imidazo[1,5-a]quinoxalin-4(5H)-one

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

Fifty (50) mg of ethyl 3-(7-chloro-4-oxo-4,5-dihydroimidazo-[1,5-a]quinoxalin-1-yl)propanoate as synthesized in Example 176 was dissolved in 5 mL of tetrahydrofuran, and to the solution 8.9 mg of lithium aluminum hydride was added under cooling with ice. After 30 minutes' stirring, the residual lithium aluminum hydride was quenched with ice pieces, and the reaction liquid was extracted with ethyl acetate. The extract was washed with saturated aqueous ammonium chloride solution, saturated aqueous sodium hydrogencarbonate solution, and with saturated brine by the order stated, and dried over anhydrous sodium sulfate. Distilling the solvent off from the product, 38 mg of the title compound was obtained.

Workup

  1. temperatureunder cooling with ice
  2. customthe residual lithium aluminum hydride was quenched with ice pieces
  3. customthe reaction liquid
  4. extractionwas extracted with ethyl acetate
  5. washThe extract was washed with saturated aqueous ammonium chloride solution, saturated aqueous sodium hydrogencarbonate solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationDistilling the solvent off from the product

Sources & evidence

ORD record
ord-616ea7670641498d80bb312f54a4bf53
Source dataset
uspto-grants-2015_05
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09040536B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes