反応 #2006433

反応方程式

4-bromo-2,2′-bipyridyl-N-oxide

PCl3

→

4-bromo-2,2′-bipyridyl

収率 85.0%

溶媒

CHCl3

反応条件

後処理

1. 1
   その他at room temperature
2. 2
   温度The mixture was refluxed for 2 h under N2
3. 3
   その他The aqueous layer was separated
4. 4
   抽出The CHCl3, layer was extracted three times with H2O (3×60 mL)
5. 5
   ろ過The resulting white precipitate was collected by suction filtration
6. 6
   洗浄washed with H2O (30 mL)
7. 7
   その他dried under vacuum at 50° C. for 24 h

実験手順

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%.

出典