反応 #701155

反応方程式

potassium ethyl xanthate

N-bromotrichloroacetamidine

→

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

収率 52.5%

溶媒

water

methylene chloride

反応条件

後処理

1. 1
   workup.ADDITIONwas added over 15 minutes
2. 2
   その他The dark methylene chloride layer was separated
3. 3
   抽出the water layer extracted with 100 ml of methylene chloride
4. 4
   乾燥The combined methylene chloride fractions were dried over magnesium sulfate
5. 5
   ろ過filtered
6. 6
   その他Next, the solvent was evaporated
7. 7
   workup.DISTILLATIONthe crude product was distilled at 75° C. under a vacuum of 0.9mm

実験手順

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.

出典