反応 #1519109

反応方程式

sodium hydride

2-cyanopyridine

urea

sulfuric acid

→

4,6-di-pyrid-2-yl-[1,3,5]triazin-2-ol

溶媒

dimethyl sulfoxide

反応条件

後処理

1. 1
   温度heated at 75° C. for 23 hours
2. 2
   温度cooled
3. 3
   ろ過the crude product is filtered off
4. 4
   その他recrystallised from 55 ml of methanol

実験手順

1.0 g (approximately 60% dispersion in paraffin oil, about 25 mmol) of sodium hydride is added in portions to a solution of 5.21 g (50 mmol) of 2-cyanopyridine and 1.50 g (25 mmol) of urea in 100 ml of dimethyl sulfoxide. The resulting suspension is maintained at room temperature for 3 hours and then heated at 75° C. for 23 hours, cooled and poured into 100 ml of ice-water. The mixture is rendered neutral with 2N sulfuric acid, and the crude product is filtered off and recrystallised from 55 ml of methanol, yielding 4,6-di-pyrid-2-yl-[1,3,5]triazin-2-ol in the form of a white solid.

出典