Ethylenediamine → HCID 176528397, Verbindung

HRID 1719354Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1719354
Cl[C:2](=[N:7][OH:8])[C:3](Cl)=[N:4][OH:5].[CH2:9]([NH2:12])[CH2:10][NH2:11]>CO>[N:4](=[C:3]1[C:2](=[N:7][OH:8])[NH:12][CH2:9][CH2:10][NH:11]1)[OH:5]

Komponenten

4

Edukt 2

HCID 3301EthylenediamineHCID 135527345Ethanediimidoyl dichloride, dihydroxy-

Produkt 1

HCID 176528397HCID 176528397, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Reaktionsbedingungen

Temperatur
5 °C

Versuchsvorschrift

Dichloroglyoxime (15.7 g, 0.10 mole) and methanol (400 ml) were placed in a one-liter, round-bottom flask. This solution was cooled to 5° C. by means of a salt-ice bath. While the solution was vigorously stirred, a solution of 12.0 g (0.20 mole) of ethylene diamine in 30 ml of methanol was added in one portion. The mixture was stirred for 10 minutes; then the solvent was removed at reduced pressure. The remaining solid was slurried with 20 ml of water and the crude 2,3-dioximinopiperazine was collected and washed with methanol. The crude product weighed 10.2 g (70%). It can be recrystallized from water (70% recovery) to give the pure compound, 2,3-dioximinopiperazine, with a melting point of 195°-196° C. (dec).

Aufarbeitung

  1. stirringThe mixture was stirred for 10 minutes
  2. customthen the solvent was removed at reduced pressure
  3. customthe crude 2,3-dioximinopiperazine was collected
  4. washwashed with methanol
  5. customIt can be recrystallized from water (70% recovery)

Quellen und Nachweise

ORD-Eintrag
ord-56f138788d8946b29ded30880144db62
Quelldatensatz
uspto-grants-1985_09
Patentnummer
US04539405

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