3-Isopropyl-2,5-piperazine-dione → 2-(Propan-2-yl)piperazine

HRID 737144

反応式

HRID 737144 の反応式
[CH:1]([CH:4]1[NH:9][C:8](=O)[CH2:7][NH:6][C:5]1=O)([CH3:3])[CH3:2].[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1>[CH:1]([CH:4]1[CH2:5][NH:6][CH2:7][CH2:8][NH:9]1)([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 1398273-Isopropyl-2,5-piperazine-dioneHCID 21226445Aluminium lithium hydride

生成物 1

HCID 5589762-(Propan-2-yl)piperazine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

2 g of 3-isopropyl-piperazine-2,5-dione could be suspended in anhydrous THF under nitrogen and cooled in an ice-bath. 4 equiv. of lithium aluminium hydride could be added. The reaction could be stirred at 0° C. for 0.5 h, then heated to reflux overnight. The reaction could be quenched by the subsequent addition of 1 mL/gLiAlH4 of water, 1 mL/gLiAlH4 of 5% aqueous sodium hydroxide solution and 3 mL/gLiAlH4 of water. The resulting solid could be separated by filtration through Celite and rinsed with ethyl acetate. The filtrate could be concentrated in vacuo to afford 2-isopropyl-piperazine.

後処理

  1. temperaturecooled in an ice-bath
  2. customThe reaction
  3. temperatureheated
  4. temperatureto reflux overnight
  5. customThe reaction
  6. customcould be quenched by the subsequent addition of 1 mL/gLiAlH4 of water, 1 mL/gLiAlH4 of 5% aqueous sodium hydroxide solution and 3 mL/gLiAlH4 of water
  7. customThe resulting solid could be separated by filtration through Celite
  8. washrinsed with ethyl acetate
  9. concentrationThe filtrate could be concentrated in vacuo

出典と根拠

ORDレコード
ord-317ed03dc2f9415daf9faf2d8f81eaab
出典データセット
uspto-grants-2009_09
特許番号
US07595397B2

関連ノート

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