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

HRID 1284620
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1284620
[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]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 20252233HCID 20252233, Verbindung

Produkt 1

HCID 202522303-[4-(Prop-2-EN-1-YL)piperazin-1-YL]propan-1-amineAusbeute 90,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

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).

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-015194ee3f7e4bb2a1ee20e2dedd116d
Quelldatensatz
uspto-grants-1986_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04563524

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