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

HRID 2389283
ノート
印刷プレビュー

反応式

HRID 2389283 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4837PiperazineHCID 684091-Chloro-2-methylpropan-2-ol

生成物 1

HCID 2582022-Methyl-1-(piperazin-1-yl)propan-2-ol収率 60%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
110 °C

実験手順

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%).

後処理

  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)

出典と根拠

ORDレコード
ord-a6bc1f669c0746ee8b14d1feff500d20
出典データセット
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08273738B2

反応ノート

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