Sodium Azide → 3-Azidoacetylpyridine
反応式
Br.Br[CH2:3][C:4]([C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1)=[O:5].[N-:12]=[N+:13]=[N-:14].[Na+].C([O-])(O)=O.[Na+]>O>[N:12]([CH2:3][C:4]([C:6]1[CH:7]=[N:8][CH:9]=[CH:10][CH:11]=1)=[O:5])=[N+:13]=[N-:14]参加物
5
実験手順
To a solution of 3-bromoacetylpyridine hydrobromide (5 g, 17.8 mmol) in 20 mL of water was added sodium azide (1.16 g, 17.8 mmol) and the contents stirred at room temperature for 2 h. The reaction mixture was treated with saturated aqueous NaHCO3 until neutrality, extracted with ethyl acetate (3×30 mL) and the combined organic phases were dried over MgSO4. After solvent removal the crude residue was silica gel column chromatographed (dichloromethane/ethanol/98/2). 3-Azidoacetyl-pyridine was obtained as yellow solid (2.17 g, 71%).
後処理
- extractionextracted with ethyl acetate (3×30 mL)
- dry with materialthe combined organic phases were dried over MgSO4
- customAfter solvent removal the crude residue
- customchromatographed (dichloromethane/ethanol/98/2)
出典と根拠
- ORDレコード
- ord-835670968c9c410ca9681e7f53c7fee4
- 出典データセット
- uspto-grants-2010_05
- 特許番号
- US07718676B2
反応ノート
読み込み中…