Sodium Hydroxide → 1,3,4-Thiadiazole, 2-amino-5-(heptylthio)-

HRID 1073781Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1073781
[NH2:1][C:2]1[S:3][C:4]([SH:7])=[N:5][N:6]=1.[OH-].[Na+].I[CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17]>O.C(O)C>[NH2:1][C:2]1[S:3][C:4]([S:7][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])=[N:5][N:6]=1

Komponenten

6

Edukt 3

HCID 14798Sodium HydroxideHCID 202741-IodoheptaneHCID 178509208HCID 178509208, Verbindung

Produkt 1

HCID 5344581,3,4-Thiadiazole, 2-amino-5-(heptylthio)-Ausbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel2×

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

In 32 ml of water and 32 ml of ethanol, 27.2 g of 2-amino-5-mercapto-1,3,4-thiadiazole and 9.0 g of sodium hydroxide were added. To this solution, 45.2 g of 1-iodoheptane was added, and the mixture was stirred at 60° C. for 2 hours. After cooling, water was added to the mixture and the mixture was filtered. The residue was washed with water, dried under reduced pressure, and recrystallized from an ethanol/n-hexane (1:1) mixture. Thus 36.1 g of 2-amino-5-heptylthio-1,3,4-thiadiazole was obtained. m.p. 112°~113° C. Yield 78%.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationthe mixture was filtered
  3. washThe residue was washed with water
  4. customdried under reduced pressure
  5. customrecrystallized from an ethanol/n-hexane (1:1) mixture

Quellen und Nachweise

ORD-Eintrag
ord-aae9ef3881284ad8809abe825254d85e
Quelldatensatz
uspto-grants-1990_11
Patentnummer
US04971971

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