반응 #701155

반응 방정식

potassium ethyl xanthate

N-bromotrichloroacetamidine

→

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

수율 52.5%

용매

water

methylene chloride

반응 조건

후처리

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

실험 절차

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.

출처