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Hydrazine hydrate (1:1) → 3-[4-(Prop-2-EN-1-YL)piperazin-1-YL]propan-1-amine

HRID 1284620
ノート
印刷プレビュー

反応式

HRID 1284620 の反応式
[CH2:1]([N:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][CH2:12][N:13]2C(=O)C3=CC=CC=C3C2=O)[CH2:6][CH2:5]1)[CH:2]=[CH2:3].O.NN>C(O)C>[CH2:1]([N:4]1[CH2:9][CH2:8][N:7]([CH2:10][CH2:11][CH2:12][NH2:13])[CH2:6][CH2:5]1)[CH:2]=[CH2:3]
参加物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 24654Hydrazine hydrate (1:1)HCID 20252233HCID 20252233、化合物

生成物 1

HCID 202522303-[4-(Prop-2-EN-1-YL)piperazin-1-YL]propan-1-amine収率 90.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of N-[3-(4-allyl-1-piperazinyl)propyl]phthalimide (35.6 g) in ethanol (400 ml) was added 100% hydrazine hydrate (14.3 g). The resulting mixture was refluxed with stirring for 2.5 hours. The reaction mixture was cooled and then filtered. The filter cake was washed with ethanol. The filtrate and washing were combined and evaporated under reduced pressure. The residual oil was subjected to column chromatigraphy (aluminum oxide), eluting with a mixture of chloroform and methanol (10:1). The fractions containing the object compound were collected and then evaporated under reduced pressure to give an oil of 3-(4-allyl-1-piperazinyl)propylamine (18.8 g).

後処理

  1. temperatureThe resulting mixture was refluxed
  2. temperatureThe reaction mixture was cooled
  3. filtrationfiltered
  4. washThe filter cake was washed with ethanol
  5. washThe filtrate and washing
  6. customevaporated under reduced pressure
  7. washeluting with a mixture of chloroform and methanol (10:1)
  8. additionThe fractions containing the object compound
  9. customwere collected
  10. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-015194ee3f7e4bb2a1ee20e2dedd116d
出典データセット
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04563524

反応ノート

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