Sodium Acetate → HCID 14989225, compound

HRID 484504Notes

Reaction equation

HRID 484504 reaction equation
Cl[C:2]1[N:7]=[N:6][C:5]([N:8]2[CH2:13][CH2:12][CH:11]([CH2:14][CH2:15][CH2:16][OH:17])[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C([O-])(=[O:20])C.[Na+]>C(O)(=O)C>[OH:17][CH2:16][CH2:15][CH2:14][CH:11]1[CH2:12][CH2:13][N:8]([C:5]2[CH:4]=[CH:3][C:2](=[O:20])[NH:7][N:6]=2)[CH2:9][CH2:10]1

Participants

4

Reactant 2

HCID 517045Sodium AcetateHCID 14989224HCID 14989224, compound

Product 1

HCID 14989225HCID 14989225, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A mixture of 6 parts of 1-(6-chloro-3-pyridazinyl)-4-piperidinepropanol, 1.9 parts of sodium acetate and 150 parts of acetic acid was stirred for 4 hours at reflex temperature. The reaction mixture was evaporated and the residue was taken up in 200 parts of a hydrochloric acid solution 10%. After stirring for 1 hour at reflux temperature, the whole was evaporated. The residue was taken up in water and treated with ammonium hydroxide. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated, yielding a first fraction of 6-[4-(3-hydroxypropyl)-1-piperidinyl]-3(2H)-pyridazinone;

Workup

  1. customThe reaction mixture was evaporated
  2. stirringAfter stirring for 1 hour
  3. temperatureat reflux temperature
  4. customthe whole was evaporated
  5. additiontreated with ammonium hydroxide
  6. extractionThe product was extracted with dichloromethane
  7. customThe extract was dried
  8. filtrationfiltered
  9. customevaporated

Sources & evidence

ORD record
ord-e666e343eda44d55b67ec9f558d610c5
Source dataset
uspto-grants-1993_07
Patent number
US05231184

Reaction notes

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