Piperazine → 2-Methyl-1-(piperazin-1-yl)propan-2-ol
Reaction equation
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[CH2:8][C:9]([CH3:12])([OH:11])[CH3:10]>C(O)C>[CH3:8][C:9]([OH:11])([CH3:12])[CH2:10][N:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 110 °C
Procedure
piperazine (6.88 g, 80.0 mmol) was dissolved in ethanol (40 mL), and 1-chloro-2-methyl-2-propanol (2.18 g, 20.0 mmol) was added thereto, and then, the mixture was stirred at 110° C. for 6 hours. After the mixture was left to cool to room temperature, the solvent was evaporated. Then, ethyl acetate was added to the residue, and the precipitated solid was removed by filtration. The solvent of the filtrate was removed under reduced pressure, and the residue was purified by silica gel column chromatography (ethyl acetate/methanol=90/10) to give 2-methyl-1-(piperazin-1-yl)propan-2-ol (1.89 g, 11.96 mmol, 60%).
Workup
- waitAfter the mixture was left
- temperatureto cool to room temperature
- customthe solvent was evaporated
- additionThen, ethyl acetate was added to the residue
- customthe precipitated solid was removed by filtration
- customThe solvent of the filtrate was removed under reduced pressure
- customthe residue was purified by silica gel column chromatography (ethyl acetate/methanol=90/10)
Sources & evidence
- ORD record
- ord-a6bc1f669c0746ee8b14d1feff500d20
- Source dataset
- uspto-grants-2012_09
- Patent number
- US08273738B2
Reaction notes
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