Reaktionsgleichung
[NH2:1][NH:2][C:3]([NH:5][NH2:6])=[S:4].[CH2:7]([O:9][CH2:10][CH2:11][C:12](O)=O)[CH3:8]>C(OCC)C>[NH2:1][N:2]1[C:12]([CH2:11][CH2:10][O:9][CH2:7][CH3:8])=[N:6][N:5]=[C:3]1[SH:4]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
63.6 g (0.6 mole) of thiocarbohydrazide and 100.0 g (0.85 mole) of 3-ethoxypropionic acid are stirred and heated at reflux until solution is achieved. The resultant solution is cooled to room temperature, diluted with 700 ml of diethyl ether and refrigerated for 1 hour. The crude white solid (94.6 g) when filtered and recrystallized from 1200 ml of water, gives 54.6 g of lustrous white plates of 4-amino-5-(2-ethoxyethyl)-4H-1,2,4-triazole-3-thiol. m.p. 123°-124° C.
Aufarbeitung
- temperatureheated
- temperatureat reflux until solution
- filtrationThe crude white solid (94.6 g) when filtered
- customrecrystallized from 1200 ml of water
Quellen und Nachweise
- ORD-Eintrag
- ord-02d4919a68c04a7d9d884e64aef163fb
- Quelldatensatz
- uspto-grants-1983_10
- Patentnummer
- US04411905
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