Potassium Hydroxide → HCID 15124609, compound
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
Product 1
Reagents, catalysts & solvents 1
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
- temperatureat reflux temperature
- customThe reaction mixture was evaporated
- additionWater was added
- extractionThe product was extracted with trichloromethane
- customThe extract was dried
- filtrationfiltered
- customevaporated
- addition2,2'-Oxybispropane was added
- filtrationThe product was filtered off
- customdried
Sources & evidence
- ORD record
- ord-417754fed8aa4dbabcbf63c44b12139e
- Source dataset
- uspto-grants-1991_03
- Patent number
- US05001125
Reaction notes
Loading…