Sodium Acetate → HCID 59606521, compound

HRID 330878Notes

Reaction equation

HRID 330878 reaction equation
Cl.Cl[C:3]1[N:8]=[N:7][C:6]([N:9]([CH3:11])[CH3:10])=[C:5]([N:12]2[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]2)[CH:4]=1.C([O-])(=O)C.[Na+]>CO.[Pd]>[CH3:10][N:9]([CH3:11])[C:6]1[N:7]=[N:8][CH:3]=[CH:4][C:5]=1[N:12]1[CH2:13][CH2:14][NH:15][CH2:16][CH2:17]1

Participants

5

Reactant 2

HCID 517045Sodium AcetateHCID 86648150HCID 86648150, compound

Product 1

HCID 59606521HCID 59606521, compound

Reagents, catalysts & solvents 2

HCID 23938PalladiumCatalystHCID 887MethanolSolvent

Procedure

9.4 g (6-chloro-4-piperazin-1-yl-pyridazin-3-yl)-dimethylamine hydrochloride and 7.3 g sodium acetate are suspended in 150 ml of methanol and hydrogenated with 1 g Pd/C 10% at ambient temperature. The catalyst is suction filtered, the filtrate is evaporated to dryness and the product is extracted with chloroform and washed with sodium hydroxide solution. The hydrochloride is precipitated with an ethereal HCl solution. 7 g (V-1) are obtained. M.p=335° C.

Workup

  1. filtrationfiltered
  2. customthe filtrate is evaporated to dryness
  3. extractionthe product is extracted with chloroform
  4. washwashed with sodium hydroxide solution
  5. customThe hydrochloride is precipitated with an ethereal HCl solution
  6. custom7 g (V-1) are obtained

Sources & evidence

ORD record
ord-4eeab4c445d74d8697482a810a111a96
Source dataset
uspto-grants-2014_11
Patent number
US08877758B2

Reaction notes

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