Hydrazine Sulfate → HCID 178485006, Verbindung

HRID 258743

Reaktionsgleichung

Reaktionsgleichung von HRID 258743
[ClH:1].Cl.O[NH:4][C:5]([NH:17][CH3:18])=[N:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16].S(O)(O)(=O)=O.[NH2:24]N.C(=O)([O-])O.[K+]>CN(C)C=O>[ClH:1].[ClH:1].[NH2:24][NH:4][C:5]([NH:17][CH3:18])=[N:6][CH2:7][CH2:8][S:9][CH2:10][C:11]1[NH:15][CH:14]=[N:13][C:12]=1[CH3:16]

Komponenten

5

Edukt 3

HCID 24842Hydrazine SulfateHCID 516893Potassium BicarbonateHCID 178485010HCID 178485010, Verbindung

Produkt 1

HCID 178485006HCID 178485006, VerbindungAusbeute 46,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
90 °C

Versuchsvorschrift

A mixture of the isothiourea dihydrochloride from Example 1 (i) (8.3 g), hydrazine sulphate (4.1 g), potassium hydrogen carbonate (12.5 g) and anhydrous dimethyl formamide (100 ml) was stirred at 90° C. for 3 hours. Following cooling and filtration from inorganic material, the filtrate containing the free base was treated with ethanolic hydrogen chloride. The residue was then triturated with isopropanol to give a solid which was recrystallised from aqueous isopropanol to give the title compound (1.94 g), m.p. 234°-235°.

Aufarbeitung

  1. temperatureFollowing cooling
  2. filtrationfiltration from inorganic material
  3. additionthe filtrate containing the free base
  4. additionwas treated with ethanolic hydrogen chloride
  5. customThe residue was then triturated with isopropanol
  6. customto give a solid which
  7. customwas recrystallised from aqueous isopropanol

Quellen und Nachweise

ORD-Eintrag
ord-2179ab7713b242788365fa0853126697
Quelldatensatz
uspto-grants-1977_07
Patentnummer
US04034101

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