Potassium Hydroxide → HCID 15124609, compound

HRID 466569Notes

Reaction equation

HRID 466569 reaction equation
[Cl:1][C:2]1[N:7]=[N:6][C:5]([N:8]2[CH2:13][CH2:12][N:11](C(OCC)=O)[CH2:10][CH2:9]2)=[CH:4][C:3]=1[CH3:19].[OH-].[K+]>C(O)CCC>[Cl:1][C:2]1[N:7]=[N:6][C:5]([N:8]2[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]2)=[CH:4][C:3]=1[CH3:19]

Participants

4

Reactant 2

HCID 14797Potassium HydroxideHCID 15124586HCID 15124586, compound

Product 1

HCID 15124609HCID 15124609, compoundYield 100%

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Procedure

A mixture of 22 parts of ethyl 4-(6-chloro-5-methyl-3-pyridazinyl)-1-piperazinecarboxylate, 28 parts of potassium hydroxide and 160 parts of 1-butanol was stirred overnight at reflux temperature. The reaction mixture was evaporated. Water was added. The product was extracted with trichloromethane. The extract was dried, filtered and evaporated. 2,2'-Oxybispropane was added. The product was filtered off and dried, yielding 17 parts (100%) of 3-chloro-4-methyl-6-(1-piperazinyl)pyridazine (compound 224).

Workup

  1. temperatureat reflux temperature
  2. customThe reaction mixture was evaporated
  3. additionWater was added
  4. extractionThe product was extracted with trichloromethane
  5. customThe extract was dried
  6. filtrationfiltered
  7. customevaporated
  8. addition2,2'-Oxybispropane was added
  9. filtrationThe product was filtered off
  10. customdried

Sources & evidence

ORD record
ord-3ad3f6efba964cd9bcf155c08af96ec6
Source dataset
uspto-grants-1992_10
Patent number
US05157035

Reaction notes

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