Potassium Hydroxide → HCID 15124609, compound

HRID 359437Notes

Reaction equation

HRID 359437 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

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-417754fed8aa4dbabcbf63c44b12139e
Source dataset
uspto-grants-1991_03
Patent number
US05001125

Reaction notes

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