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Hydrazine → HCID 21515433, Verbindung

HRID 1284329
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1284329
[Cl:1][C:2]1[N:3]=[N:4][CH:5]=[C:6]([NH2:8])[CH:7]=1.[NH2:9][NH2:10]>>[ClH:1].[ClH:1].[NH2:8][C:6]1[CH:7]=[C:2]([NH:9][NH2:10])[N:3]=[N:4][CH:5]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

3

Edukt 2

HCID 9321HydrazineHCID 140991445-Amino-3-chloro-pyridazine

Produkt 1

HCID 21515433HCID 21515433, Verbindung

Versuchsvorschrift

7 g. of 3-chloro-5-aminopyridazine is added to 125 ml. of hydrazine and the mixture is stirred under nitrogen for 17.5 hours at a temperature below reflux. The reaction mixture is cooled to room temperature, and the residual hydrazine removed by evaporation. The residue is treated with 250 ml. of methanol to extract the product. After separating the extractant and washing the residue with small amounts of methanol, the combined extractant-filtrate is treated with hydrogen chloride gas. The solution is then treated with ether to give a crystalline product which is recrystallized from methanol to give 5-amino-3-hydrazinopyridazine dihydrochloride; m.p. 220°-222°C.

Aufarbeitung

  1. temperaturebelow reflux
  2. customthe residual hydrazine removed by evaporation
  3. additionThe residue is treated with 250 ml
  • extractionof methanol to extract the product
  • customAfter separating the extractant
  • washwashing the residue with small amounts of methanol
  • additionthe combined extractant-filtrate is treated with hydrogen chloride gas
  • additionThe solution is then treated with ether
  • customto give a crystalline product which
  • customis recrystallized from methanol
  • Quellen und Nachweise

    ORD-Eintrag
    ord-e230a57f9374441daf7af5200a81fe3b
    Quelldatensatz
    uspto-grants-1976_08
    DOI
    10.6084/m9.figshare.5104873.v1
    Patentnummer
    US03978057

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