Sodium methanolate methanol → HCID 58201209, compound

HRID 2093548Notes

Reaction equation

HRID 2093548 reaction equation
[CH3:1][O-:2].[Na+].CO.[Br:6][C:7]1[C:8]([N+]([O-])=O)=[C:9]([CH3:15])[C:10]([CH3:14])=[N+:11]([O-:13])[CH:12]=1>CO>[Br:6][C:7]1[C:8]([O:2][CH3:1])=[C:9]([CH3:15])[C:10]([CH3:14])=[N+:11]([O-:13])[CH:12]=1

Participants

4

Procedure

A 1 M sodium methoxide-methanol solution (30 ml) was added to a methanol (20 ml) solution of the above 5-bromo-2,3-dimethyl-4-nitropyridine 1-oxide (4.80 g) under cooling in an ice bath, and the resulting mixture was stirred at room temperature overnight. Thereafter, the reaction solution was concentrated, and the residue was dissolved in dichloromethane and water for liquid separation. The organic layer was dried over anhydrous sodium sulfate, and the filtrate was then concentrated, so as to obtain a crude product of the title compound (4.91 g) as a solid.

Workup

  1. temperatureunder cooling in an ice bath
  2. concentrationThereafter, the reaction solution was concentrated
  3. dissolutionthe residue was dissolved in dichloromethane
  4. customwater for liquid separation
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. concentrationthe filtrate was then concentrated

Sources & evidence

ORD record
ord-80a0a59a11cf40b4b8e3c60a46d07dbc
Source dataset
uspto-grants-2013_05
Patent number
US08445504B2

Reaction notes

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