反応式
[C:1]([CH2:3][C:4]1[CH:5]=[N+:6]([O-])[CH:7]=[CH:8][CH:9]=1)#[N:2].C[Si](C)(C)[C:13]#[N:14].CN(C)C(Cl)=O>ClCCl>[C:13]([C:5]1[C:4]([CH2:3][C:1]#[N:2])=[CH:9][CH:8]=[CH:7][N:6]=1)#[N:14]参加物
5
実験手順
To a stirred suspension of 3-cyanomethylpyridine-N-oxide (30 g, 0.22 mol; for synthesis see Shigenobu Okuda, Michael M. Robison, J. Am. Chem. Soc. 81, 740 (1959)) in dichloromethane (200 ml) is added trimethylsilanecarbonitrile (26 g, 0.26 mol). To this suspension is added dimethylcarbamyl chloride (28 g, 0.26 mol). The mixture is stirred for 45 h. The solvent is removed and the residue dissolved in ethyl acetate. The solution is washed with 1 N NaOH and water and concentrated in vacuo. The product is purified by flash column chromatography on silica gel (15:2 toluene/acetone) affording the title compound. Mass M+H 144.1. Melting point 62-63° C.
後処理
- customThe solvent is removed
- dissolutionthe residue dissolved in ethyl acetate
- washThe solution is washed with 1 N NaOH and water
- concentrationconcentrated in vacuo
- customThe product is purified by flash column chromatography on silica gel (15:2 toluene/acetone)
出典と根拠
- ORDレコード
- ord-902b28c48d864fa98c2458152f224f06
- 出典データセット
- uspto-grants-2000_10
- 特許番号
- US06136821
関連ノート
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