Piperazine → 2-Methyl-1-(piperazin-1-yl)propan-2-ol

HRID 2389283Notes

Reaction equation

HRID 2389283 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]1

Participants

4

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

  1. waitAfter the mixture was left
  2. temperatureto cool to room temperature
  3. customthe solvent was evaporated
  4. additionThen, ethyl acetate was added to the residue
  5. customthe precipitated solid was removed by filtration
  6. customThe solvent of the filtrate was removed under reduced pressure
  7. 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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