Sodium Acetate → HCID 59606521, compound

HRID 408091Notes

Reaction equation

HRID 408091 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-861c9b4611664d34a4e3485d8970c31f
Source dataset
uspto-grants-2014_06
Patent number
US08759326B2

Reaction notes

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