Piperazine → HCID 70480299, compound
Reaction equation
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:7]([OH:14])(=[O:13])/[CH:8]=[CH:9]\[C:10]([OH:12])=[O:11]>C(O)C>[C:7]([OH:14])(=[O:13])/[CH:8]=[CH:9]\[C:10]([OH:12])=[O:11].[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1Participants
4
Reagents, catalysts & solvents 1
Procedure
Monomaleate salt--5 g. (0.0115 mole) of 1-diphenylmethyl-4-[2-(-4-methylphenyl)-5-methyl-1H-imidazol-4-yl)-methyl]piperazine were dissolved in 300 ml of ethanol at 95° C. To this solution 1.34 g (0.0115 mole) of maleic acid was added with stirring. The reaction mixture was stirred at room temperature for 2 hours then the solvents were evaporated off under reduced pressure. The residue was dissolved in ether and the precipitate was filtered. The precipitate was recrystallized from isopropyl ether:acetone (1:1) to yield 1-diphenylmethyl-4-[2-(-4-methylphenyl)-5-methyl-1H-imidazol-4-yl)-methyl]piperazine monomaleate, m.p. 164°-166° C. with decomposition.
Workup
- stirringThe reaction mixture was stirred at room temperature for 2 hours
- customthe solvents were evaporated off under reduced pressure
- dissolutionThe residue was dissolved in ether
- filtrationthe precipitate was filtered
- customThe precipitate was recrystallized from isopropyl ether:acetone (1:1)
Sources & evidence
- ORD record
- ord-ec44805178f3404895bdaf609c4914e1
- Source dataset
- uspto-grants-1991_08
- Patent number
- US05043447
Reaction notes
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