반응 #2006433

반응 방정식

4-bromo-2,2′-bipyridyl-N-oxide

PCl3

→

4-bromo-2,2′-bipyridyl

수율 85.0%

용매

CHCl3

반응 조건

후처리

1. 1
   기타at room temperature
2. 2
   온도The mixture was refluxed for 2 h under N2
3. 3
   기타The aqueous layer was separated
4. 4
   추출The CHCl3, layer was extracted three times with H2O (3×60 mL)
5. 5
   여과The resulting white precipitate was collected by suction filtration
6. 6
   세척washed with H2O (30 mL)
7. 7
   기타dried under vacuum at 50° C. for 24 h

실험 절차

To a stirred suspension of 4-bromo-2,2′-bipyridyl-N-oxide in 60 mL CHCl3, was added 12 mL PCl3, at room temperature. The mixture was refluxed for 2 h under N2 and then cooled to room temperature. The reaction mixture was poured into 100 mL ice/water. The aqueous layer was separated and saved. The CHCl3, layer was extracted three times with H2O (3×60 mL) and then discarded. The combined aqueous solution was neutralized with NaHCO3 powder to about pH 7-8. The resulting white precipitate was collected by suction filtration, washed with H2O (30 mL) and then dried under vacuum at 50° C. for 24 h. Yield: 85%.

출처