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Hydrazine hydrate (1:1) → 3-(4-Isopropyl-piperazin-1-yl)-propylamine

HRID 1284627
ノート
印刷プレビュー

反応式

HRID 1284627 の反応式
[CH: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)([CH3:3])[CH3:2].O.NN>C(O)C>[CH:1]([N:4]1[CH2:5][CH2:6][N:7]([CH2:10][CH2:11][CH2:12][NH2:13])[CH2:8][CH2:9]1)([CH3:3])[CH3:2]
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 20252235N-[3-(4-isopropyl-1-piperazinyl)propyl]phthalimide

生成物 1

HCID 128029563-(4-Isopropyl-piperazin-1-yl)-propylamine収率 59.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of N-[3-(4-isopropyl-1-piperazinyl)propyl]phthalimide (43.1 g) in ethanol (350 ml) was added 100% hydrazine hydrate (11.2 g). The resulting mixture was refluxed with stirring for 3 hours. The reaction mixture was cooled and then filtered. The filter cake was washed with ethanol. The filtrate and washing were combined and concentrated under reduced pressure. The residual oil was subjected to column chromatography (aluminum oxide), eluting with a mixture of chloroform and methanol (20:1). The fractions containing the object compound were collected and then evaporated under reduced pressure. The residual oil was distilled under reduced pressure to give 3-(4-isopropyl-1-piperazinyl)propylamine (15.0 g), (bp 45 mmHg/150° C.).

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. concentrationconcentrated under reduced pressure
  7. washeluting with a mixture of chloroform and methanol (20:1)
  8. additionThe fractions containing the object compound
  9. customwere collected
  10. customevaporated under reduced pressure
  11. distillationThe residual oil was distilled under reduced pressure

出典と根拠

ORDレコード
ord-de84a78453be4cba959090a31cb1c7f4
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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