反応 #461936

反応方程式

3-chloro-4-(2,6-dichlorophenyl)-1,2,5-thiadiazole

methylamine

→

3-(2,6-dichlorophenyl)-4-methylamino-1,2,5-thiadiazole

溶媒

water

反応条件

後処理

1. 1
   温度to cool
2. 2
   抽出was extracted With ether
3. 3
   洗浄The ether layer was washed three times with water and three times with saturated aqueous sodium chloride solution
4. 4
   乾燥The resultant was then dried over anhydrous sodium sulfate
5. 5
   濃縮the resultant was concentrated
6. 6
   その他followed by purification by silica gel column chromatography

実験手順

In a stainless steel vessel, 5.31 g of 3-chloro-4-(2,6-dichlorophenyl)-1,2,5-thiadiazole and 100 ml of 40% aqueous methylamine solution were placed. After sealing the vessel, the solution was stirred at 120° C. for 12 hours. After allowing to cool, the mixture was poured into water and was extracted With ether. The ether layer was washed three times with water and three times with saturated aqueous sodium chloride solution. The resultant was then dried over anhydrous sodium sulfate and then the resultant was concentrated, followed by purification by silica gel column chromatography to obtain 2.55 g of 3-(2,6-dichlorophenyl)-4-methylamino-1,2,5-thiadiazole.

出典