반응 #1519109
ord-86efa83661164abdb84768abe242acfb
반응 방정식
sodium hydride
2-cyanopyridine
urea
sulfuric acid
→
4,6-di-pyrid-2-yl-[1,3,5]triazin-2-ol
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도heated at 75° C. for 23 hours
- 2온도cooled
- 3여과the crude product is filtered off
- 4기타recrystallised from 55 ml of methanol
실험 절차
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.