Methanol → 1,4-Di(n-butyl)piperazin-2-one

HRID 35732

反応式

HRID 35732 の反応式
[CH:1]([CH:3]=O)=[O:2].CO.[CH2:7]([NH:11][CH2:12][CH2:13][NH:14][CH2:15][CH2:16][CH2:17][CH3:18])[CH2:8][CH2:9][CH3:10]>O1CCOCC1>[CH2:15]([N:14]1[CH2:13][CH2:12][N:11]([CH2:7][CH2:8][CH2:9][CH3:10])[CH2:3][C:1]1=[O:2])[CH2:16][CH2:17][CH3:18]

参加物

5

反応物 3

HCID 887MethanolHCID 7860GlyoxalHCID 77629N,N'-Dibutylethylenediamine

生成物 1

HCID 142506501,4-Di(n-butyl)piperazin-2-one収率 30.7%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To 10 g (69.0 mmoles) of 40 percent glyoxal and 200 ml of methanol is rapidly added 11.9 g (69.0 mmoles) of N,N'-di(n-butyl)ethylenediamine. The solution is rapidly brought to reflux and heating is maintained for 5 minutes. The dark brown solution is then allowed to cool to room temperature at which time fine white crystals precipitate from the brown oil. The oil is diluted with 100 ml of 1,4-dioxane and the solid is removed by filtration. The dioxane solution is concentrated under aspirator vacuum and distilled in a short path distillation apparatus to give 4.5 g of 1,4-di(n-butyl)piperazin-2-one in the form of a brown oil (31 percent yield).

後処理

  1. temperatureto reflux
  2. temperatureheating
  3. temperatureis maintained for 5 minutes
  4. customthe solid is removed by filtration
  5. concentrationThe dioxane solution is concentrated under aspirator vacuum
  6. distillationdistilled in a short path distillation apparatus

出典と根拠

ORDレコード
ord-94d3d49cf1044e7883ab64fe7800a8d7
出典データセット
uspto-grants-1988_08
特許番号
US04767860

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