Reaktion #1160996

Reaktionsgleichung

2,5-dimercapto-1,3,4-thiadiazole

sodium hydroxide

N,N-dimethylchloroacetamidine

→

2-(N,N-dimethylamidinomethylthio)-5-mercapto-1,3,4-thiadiazole

Ausbeute 53.3%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added to the suspension
2. 2
   workup.STIRRINGThe mixture was stirred at room temperature for an hour
3. 3
   Einengenconcentrated under reduced pressure
4. 4
   FiltrationThe precipitating crystals were collected by filtration
5. 5
   Waschenwashed with cold water
6. 6
   workup.ADDITIONa (1:1) mixture of methanol and ethyl ether

Vorschrift

In 30 ml of ethanol was suspended 2.25 g of 2,5-dimercapto-1,3,4-thiadiazole, and 30 ml of 1N-sodium hydroxide solution was added to the suspension. The mixture was stirred at room temperature for 30 minutes. To the mixture was added 2.36 g of N,N-dimethylchloroacetamidine. The mixture was stirred at room temperature for an hour and concentrated under reduced pressure. The precipitating crystals were collected by filtration and washed with cold water and then a (1:1) mixture of methanol and ethyl ether to obtain 1.87 g of 2-(N,N-dimethylamidinomethylthio)-5-mercapto-1,3,4-thiadiazole as colorless crystals (mp 95°-97° C.).

Quelle