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Sulfuric Acid → 2-Bromo-12H-chromeno[2,3-b]quinolin-12-one

HRID 2046091
Notes
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Reaction equation

HRID 2046091 reaction equation
[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][C:7]([NH:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)=[C:6]([CH:19]=O)[C:5]2=[O:21].OS(O)(=O)=O>>[Br:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[O:8][C:7]1=[N:12][C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[CH:19]=[C:6]1[C:5]2=[O:21]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

3

Reactant 2

HCID 1118Sulfuric AcidHCID 866606206-Bromo-4-oxo-2-(phenylamino)-4H-chromene-3-carbaldehyde

Product 1

HCID 666150262-Bromo-12H-chromeno[2,3-b]quinolin-12-oneYield 77%

Procedure

To the product of Step A (1 g; 2.92 mmol) concentrated H2SO4 (1 ml) was gently added with stirring. The mixture was kept in sealed vial for 24 h, at room temperature, than poured onto ice water and extracted with CH2Cl2 (50 ml). The organic layer was washed with NaHCO3 solution, H2O, dried over MgSO4 and filtered. The filtrate was distilled off and the residue was crystallized from CH3CN to give the title compound (0.73 g, 77%), as green yellow solid. 1H-NMR (CDCl3) 9.28 (s, 1H); 8.44 (d, 1H, J=2.1 Hz); 8.1-8.06 (m, 2H); 7.94-7.84 (m, 2H); 7.63 (t, 1H, J=7.88 Hz); 7.51 (d, 1H, J=8.83 Hz).

Workup

  1. custom
sealed vial for 24 h
  • additionat room temperature, than poured onto ice water
  • extractionextracted with CH2Cl2 (50 ml)
  • washThe organic layer was washed with NaHCO3 solution, H2O
  • dry with materialdried over MgSO4
  • filtrationfiltered
  • distillationThe filtrate was distilled off
  • customthe residue was crystallized from CH3CN
  • Sources & evidence

    ORD record
    ord-1bdd102b1c54469d9c23811731fe6760
    Source dataset
    uspto-grants-2013_11
    DOI
    10.6084/m9.figshare.5104873.v1
    Patent number
    US08592399B2

    Reaction notes

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    On this pageParticipantsProcedureWorkupSources & evidenceReaction notes