Hydrazine → 1-(2-Hydroxyethyl)-2-hydrazinoimidazoline mesylate

HRID 256542

Reaktionsgleichung

Reaktionsgleichung von HRID 256542
[S:1]([OH:5])(=[O:4])(=[O:3])[CH3:2].[OH:6][CH2:7][CH2:8][N:9]1[CH2:13][CH2:12][N:11]=[C:10]1SC.[NH2:16][NH2:17]>C(O)C.COC(C)(C)C>[S:1]([OH:5])(=[O:4])(=[O:3])[CH3:2].[OH:6][CH2:7][CH2:8][N:9]1[CH2:13][CH2:12][N:11]=[C:10]1[NH:16][NH2:17]

Komponenten

5

Edukt 2

HCID 9321HydrazineHCID 197853791-(2-Hydroxyethyl)-2-methylthioimidazoline mesylate

Produkt 1

HCID 197854081-(2-Hydroxyethyl)-2-hydrazinoimidazoline mesylate

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 15413tert-Butyl methyl etherLösungsmittel

Versuchsvorschrift

1-(2-Hydroxyethyl)-2-methylthioimidazoline mesylate (35 g, 0.136 mole) is suspended in ethyl alcohol (80 ml) and treated with anhydrous hydrazine (9.3 ml, 0.296 mole). The mixture became clear immediately. The solution is stirred at room temperature overnight and then diluted with t-butyl methyl ether (1 liter). On storage of the mixture in the freezer at -20° C., crystals separated, which are filtered, washed well with t-butyl methyl ether and dried. Recrystallization from isopropyl alcohol and t-butyl methyl ether gives 1-(2-hydroxyethyl)-2-hydrazinoimidazoline mesylate, melting point 85°-88° C.

Aufarbeitung

  1. customOn storage of the mixture in the freezer at -20° C., crystals separated
  2. filtrationwhich are filtered
  3. washwashed well with t-butyl methyl ether
  4. customdried
  5. customRecrystallization from isopropyl alcohol and t-butyl methyl ether

Quellen und Nachweise

ORD-Eintrag
ord-c9809d95a10348d3ab8f28f924a495e8
Quelldatensatz
uspto-grants-1993_11
Patentnummer
US05258381

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