Sodium Methoxide → HCID 68698216, compound

HRID 2244353Notes

Reaction equation

HRID 2244353 reaction equation
Cl[C:2]1[N:7]=[N:6][C:5]([NH:8][CH3:9])=[C:4]([C:10]([OH:12])=[O:11])[CH:3]=1.[CH3:13][O-:14].[Na+]>CO>[CH3:13][O:14][C:2]1[N:7]=[N:6][C:5]([NH:8][CH3:9])=[C:4]([C:10]([OH:12])=[O:11])[CH:3]=1

Participants

4

Reactant 2

HCID 10942334Sodium MethoxideHCID 86615233HCID 86615233, compound

Product 1

HCID 68698216HCID 68698216, compoundYield 22%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A solution of 6-chloro-3-methylamino-pyridazine-4-carboxylic acid (80 mg, 0.43 mmol), sodium methoxide solution (5.4 M in methanol, 1.0 mL, 5.4 mmol) in methanol (1 mL) was heated at 170° C. for 20 min. After cooling, the solution was evaporated, the residue dissolved in water (2 mL) and acidified to pH 3 by addition of 37% aq. hydrochloric acid solution. The precipitate was collected by filtration to afford the title compound (17 mg, 22%). White solid, MS (ISP): 182.1 (M−H)−.

Workup

  1. temperatureAfter cooling
  2. customthe solution was evaporated
  3. dissolutionthe residue dissolved in water (2 mL)
  4. additionacidified to pH 3 by addition of 37% aq. hydrochloric acid solution
  5. filtrationThe precipitate was collected by filtration

Sources & evidence

ORD record
ord-cf8246b036bf4676a608f164b4d3ea74
Source dataset
uspto-grants-2010_03
Patent number
US07678818B2

Reaction notes

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