Methanol → HCID 18629200, compound

HRID 1060573Notes

Reaction equation

HRID 1060573 reaction equation
[CH3:1][O-:2].[Na+].[Na].Cl[C:6]1[C:15](Cl)=[N:14][C:13]2[C:8](=[CH:9][C:10]([N+:18]([O-:20])=[O:19])=[C:11]([F:17])[CH:12]=2)[N:7]=1.[CH3:21][OH:22]>>[CH3:1][O:2][C:6]1[C:15]([O:22][CH3:21])=[N:14][C:13]2[C:8](=[CH:9][C:10]([N+:18]([O-:20])=[O:19])=[C:11]([F:17])[CH:12]=2)[N:7]=1

Participants

5

Procedure

To a solution of sodium methoxide which was prepared from dried methanol 75 mL and metallic sodium 1.332 g, was added 2,3-dichloro-6-fluoro-7-nitroquinoxaline 4.778 g under ice-cooling and the mixture was stirred at room temperature for 1 hr. The reaction mixture was poured into ice water, then the resulting precipitation was collected and washed with water. The aqueous layer was extracted with chloroform, then the combined product was purified with alumina column chromatography and crystallized from acetone/hexane, to give the title compound (white crystal) 3.342 g.

Workup

  1. temperaturecooling
  2. customthe resulting precipitation
  3. customwas collected
  4. washwashed with water
  5. extractionThe aqueous layer was extracted with chloroform
  6. customthe combined product was purified with alumina column chromatography
  7. customcrystallized from acetone/hexane

Sources & evidence

ORD record
ord-ce1326d340e94b6c90a909caa46d1a6a
Source dataset
uspto-grants-2003_02
Patent number
US06525054B1

Reaction notes

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