Sodium Hydroxide → 2-Bromo-3,3'-bipyridine
反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([C:7]2[C:8](=O)[NH:9][CH:10]=[CH:11][CH:12]=2)[CH:2]=1.[OH-].[Na+].P(Br)(Br)([Br:18])=O>>[Br:18][C:8]1[C:7]([C:3]2[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=2)=[CH:12][CH:11]=[CH:10][N:9]=1参加物
4
実験手順
A mixture of 0.30 g of 3-(3-pyridinyl)-2(1H)pyridinone and 10 ml of phosphorus oxybromide was heated on a steam bath for 18 hours, then poured onto crushed ice and made alkaline with 10N sodium hydroxide. The resulting solid was collected, dissolved in methylene chloride and the solution passed through a short pad of hydrous magnesium silicate. The filtrate was concentrated and while boiling diluted with hexane. Concentration and chilling gave 2'-bromo-3,3'-bipyridine as white crystals, mp 97°-98° C.
後処理
- temperaturewas heated on a steam bath for 18 hours
- additionpoured
- customonto crushed ice
- customThe resulting solid was collected
- dissolutiondissolved in methylene chloride
- concentrationThe filtrate was concentrated
- additionwhile boiling diluted with hexane
- concentrationConcentration
- temperaturechilling
出典と根拠
- ORDレコード
- ord-b11575c0cb7548709b94151f7fc3e5c5
- 出典データセット
- uspto-grants-1985_10
- 特許番号
- US04550166
反応ノート
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