Methanol → HCID 178481705, Verbindung

HRID 444555

Reaktionsgleichung

Reaktionsgleichung von HRID 444555
[C:1]([NH:5][NH2:6])(=O)[CH2:2][OH:3].[CH3:7][N:8]=[C:9]=[S:10].CO.[Na]>C(O)C>[OH:3][CH2:2][C:1]1[N:8]([CH3:7])[C:9]([SH:10])=[N:6][N:5]=1

Komponenten

6

Edukt 4

HCID 887MethanolHCID 11167Methyl isothiocyanateHCID 3505362-HydroxyacetohydrazideHCID 5360545Sodium

Produkt 1

HCID 178481705HCID 178481705, VerbindungAusbeute 35,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 9 g of glycolic acid hydrazide, 7.3 g of methyl isothiocyanate, 50 ml of methanol and 50 ml of ethanol was heated under reflux for 5 hours. Following the addition of 2.3 g of sodium metal, the mixture was further refluxed for 24 hours. The reaction mixture was concentrated under reduced pressure and the residue was dissolved in 150 ml of water and adjusted to pH 2.5 with phosphoric acid. The resultant crystals were collected by filtration and recrystallized from ethanol. By the above procedure there were obtained 5.2 g of the captioned compound. m.p. 199°-201° C.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours
  3. temperaturethe mixture was further refluxed for 24 hours
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. dissolutionthe residue was dissolved in 150 ml of water
  6. filtrationThe resultant crystals were collected by filtration
  7. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-2a9cfc64dc5e44e7a2c3edc3180ea0a0
Quelldatensatz
uspto-grants-1981_04
Patentnummer
US04264595

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