Sodium Azide → 3-Azidoacetylpyridine
반응식
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]참가 물질
5
실험 절차
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%).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-835670968c9c410ca9681e7f53c7fee4
- 출처 데이터셋
- uspto-grants-2010_05
- 특허 번호
- US07718676B2
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