Methyl iodide → 6-methoxy-1H-pyrrolo[2,3-b]pyridine
反応式
[NH:1]1[C:5]2=[N:6][C:7]([OH:10])=[CH:8][CH:9]=[C:4]2[CH:3]=[CH:2]1.[C:11]([O-])([O-])=O.[K+].[K+].CI>CC(C)=O>[CH3:11][O:10][C:7]1[N:6]=[C:5]2[NH:1][CH:2]=[CH:3][C:4]2=[CH:9][CH:8]=1参加物
5
実験手順
A mixture of 1H-pyrrolo[2,3-b]pyridin-6-ol (0.200 g, 1.49 mmol) and K2CO3 (1 g, 7.45 mmol) in acetone (30 mL) was stirred under N2 at room temperature for 1 h. MeI (0.166 g, 1.192 mmol) was added. The reaction mixture was stirred under N2 at 50° C. for 12 h and then filtered. The filtrate was concentrated to half its volume, diluted with water, and extracted with CH2Cl2. The organic layer was dried over anhydrous MgSO4, and evaporated to give a residue, which was purified on a column of silica gel eluting with EtOAc/hexane (1:4) to give 6-methoxy-1H-pyrrolo[2,3-b]pyridine (159 mg, 89%).
後処理
- stirringThe reaction mixture was stirred under N2 at 50° C. for 12 h
- filtrationfiltered
- concentrationThe filtrate was concentrated to half its volume
- additiondiluted with water
- extractionextracted with CH2Cl2
- dry with materialThe organic layer was dried over anhydrous MgSO4
- customevaporated
- customto give a residue, which
- customwas purified on a column of silica gel eluting with EtOAc/hexane (1:4)
出典と根拠
- ORDレコード
- ord-6491a58bc9574c9da7db5d60ee9f6eb1
- 出典データセット
- uspto-grants-2008_11
- 特許番号
- US07456289B2
反応ノート
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