Sodium Acetate → 4-(Piperazin-1-yl)pyridazine
Reaction equation
Cl[C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1.C([O-])(=O)C.[Na+]>CO.[Pd]>[N:8]1([C:7]2[CH:6]=[CH:5][N:4]=[N:3][CH:2]=2)[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]1Participants
5
Reactant 2
Product 1
Reagents, catalysts & solvents 2
Procedure
9.3 g 3,6-dichloro-4-piperazin-1-yl-pyridazine (see 10.2) and 6.5 g sodium acetate are suspended in 100 ml of methanol and hydrogenated with 1 g Pd/C 10% and ambient temperature. The catalyst is suction filtered and the filtrate is evaporated to dryness. The product is extracted with chloroform, washed with sodium hydroxide solution and precipitated as the hydrochloride with an ethereal HCl solution. 8.6 g (V-4) are obtained. M.p>300° C.
Workup
- filtrationfiltered
- customthe filtrate is evaporated to dryness
- extractionThe product is extracted with chloroform
- washwashed with sodium hydroxide solution
- customprecipitated as the hydrochloride with an ethereal HCl solution
- custom8.6 g (V-4) are obtained
- customM.p>300° C.
Sources & evidence
- ORD record
- ord-b1314ee7cc7a4e4487e547c70944bd0d
- Source dataset
- uspto-grants-2015_08
- Patent number
- US09115142B2
Reaction notes
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