Water → HCID 54731250, compound

HRID 2166331Notes

Reaction equation

HRID 2166331 reaction equation
[OH2:1].[Cl:2][C:3]1[C:4](=[O:14])[N:5]([CH2:10][CH2:11][CH2:12][OH:13])[N:6]=[CH:7][C:8]=1Cl.[OH-].[K+]>C(O)C>[Cl:2][C:3]1[C:4](=[O:14])[N:5]([CH2:10][CH2:11][CH2:12][OH:13])[N:6]=[CH:7][C:8]=1[OH:1]

Participants

5

Reactant 3

HCID 962WaterHCID 14797Potassium HydroxideHCID 23039514HCID 23039514, compound

Product 1

HCID 54731250HCID 54731250, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent2×

Procedure

To a mixed solvent of 150 ml of water and 150 ml of ethanol was added 22.3 g of 4,5-dichloro-2-(3'-hydroxypropyl)-3(2H)-pyridazinone (0.1 mol) and 19.6 g of potassium hydroxide (0.35 mol) and then heated under reflux for about 10 hours. After reaction, ethanol was removed under reduced pressure and added with water to filter off the insoluble matters. The filtrate was converted into acidity by diluted hydrochloric acid and the crystals produced were filtered off. The crystals thus obtained were washed with water and dried to give 14.5 g of 4-chloro-5-hydroxy-2-(3'-hydroxypropyl)-3(2H)-pyridazinone.

Workup

  1. temperatureheated
  2. temperatureunder reflux for about 10 hours
  3. customwas removed under reduced pressure
  4. additionadded with water
  5. filtrationto filter off the insoluble matters
  6. customthe crystals produced
  7. filtrationwere filtered off
  8. customThe crystals thus obtained
  9. washwere washed with water
  10. customdried

Sources & evidence

ORD record
ord-d6902d05a2764e28b2196683986ca785
Source dataset
uspto-grants-1990_07
Patent number
US04945091

Reaction notes

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