反応 #56387

反応方程式

cyanuric chloride

cyclopropylamine

sodium hydroxide

→

2-cyclopropylamino-4,6-dichloro-s-triazine

溶媒

chlorobenzene

反応条件

後処理

1. 1
   workup.ADDITIONTo this suspension are added
2. 2
   その他at -10° C.
3. 3
   workup.WAITto stand for a further 16 hours at room temperature
4. 4
   洗浄after which it is washed with water (2×400 ml)
5. 5
   乾燥dried over anhydrous sodium sulphate
6. 6
   ろ過filtered
7. 7
   その他The excess chlorobenzene is then removed by water jet vacuum distillation

実験手順

133 g of cyanuric chloride are suspended in 720 ml of chlorobenzene and cooled to -10° C. To this suspension are added with stirring 50 ml of cyclopropylamine dropwise over a period of 25 minutes. Keeping the temperature at -10° C., 96 ml of aqueous sodium hydroxide (30% NaOH) are added dropwise. The reaction mixture is then stirred at -10° C. for 11/2 hours and allowed to stand for a further 16 hours at room temperature, after which it is washed with water (2×400 ml), dried over anhydrous sodium sulphate and filtered. The excess chlorobenzene is then removed by water jet vacuum distillation. 138 g of 2-cyclopropylamino-4,6-dichloro-s-triazine in the form of white crystals are obtained.

出典