Sodium Cyanide → (6-Methoxypyridin-3-yl)acetonitrile
反応式
[C-:1]#[N:2].[Na+].Cl[CH2:5][C:6]1[CH:7]=[CH:8][C:9]([O:12][CH3:13])=[N:10][CH:11]=1>CS(C)=O.[Cl-].[Na+].O>[CH3:13][O:12][C:9]1[N:10]=[CH:11][C:6]([CH2:5][C:1]#[N:2])=[CH:7][CH:8]=1参加物
5
実験手順
Sodium cyanide (1.25 g, 25.4 mmol) was added to a solution of 5-(chloromethyl)-2-methoxypyridine (1.00 g, 6.34 mmol) in DMSO (10 ml) and stirred for 18 h at room temperature. After completion of reaction, the reaction mixture was diluted with brine and the compound was extracted with DCM (3×35 ml). The combined organic layers were dried over anhydrous sodium sulfate, filtered and evaporated. The crude compound was purified by column chromatography using 100-200 silica gel, 10% ethyl acetate in petroleum ether as eluent to afford 0.6 g (63.8%) of 2-(6-methoxypyridin-3-yl)acetonitrile as white color solid.
後処理
- customAfter completion of reaction
- extractionthe compound was extracted with DCM (3×35 ml)
- dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
- filtrationfiltered
- customevaporated
- customThe crude compound was purified by column chromatography
出典と根拠
- ORDレコード
- ord-7c2a6a92ed3944848e74570f3cbf7533
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08518948B2
反応ノート
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