Reaktion #701155

Reaktionsgleichung

potassium ethyl xanthate

N-bromotrichloroacetamidine

→

3-trichloromethyl-5-ethoxy-1,2,4-thiadiazole

Ausbeute 52.5%

Lösungsmittel

water

methylene chloride

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONwas added over 15 minutes
2. 2
   SonstigeThe dark methylene chloride layer was separated
3. 3
   Extraktionthe water layer extracted with 100 ml of methylene chloride
4. 4
   TrocknenThe combined methylene chloride fractions were dried over magnesium sulfate
5. 5
   Filtrationfiltered
6. 6
   SonstigeNext, the solvent was evaporated
7. 7
   workup.DISTILLATIONthe crude product was distilled at 75° C. under a vacuum of 0.9mm

Vorschrift

32 g (0.2 mole) of potassium ethyl xanthate was dissolved in 175 ml of water. This was stirred rapidly while a solution of 48 g (0.2 mole) of N-bromotrichloroacetamidine in 150 ml of methylene chloride was added over 15 minutes. Then, the mixture was stirred one hour at room temperature. The dark methylene chloride layer was separated and the water layer extracted with 100 ml of methylene chloride. The combined methylene chloride fractions were dried over magnesium sulfate and filtered. Next, the solvent was evaporated and then the crude product was distilled at 75° C. under a vacuum of 0.9mm to give 26 g of 3-trichloromethyl-5-ethoxy-1,2,4-thiadiazole.

Quelle