Cyclopentanone → 1-(Dimethylamino)cyclopentanecarbonitrile
反応式
Cl.[CH3:2][NH:3][CH3:4].[C:5]1(=O)[CH2:9][CH2:8][CH2:7][CH2:6]1.[C-:11]#[N:12].[K+]>O>[CH3:2][N:3]([CH3:4])[C:5]1([C:11]#[N:12])[CH2:9][CH2:8][CH2:7][CH2:6]1参加物
5
実験手順
To a suspension of dimethylamine hydrochloride (8.15 g; 0.1 mol) in cyclopentanone (8.4 g; 0.1 mol) cooled (ice bath) was added dropwise a solution of potassium cyanide (6.5 g; 0.1 mol) in water (50 ml) over 10 min. After vigorous stirring at room temperature for 18 h, the crude reaction mixture was extracted three times with diethyl ether (3×200 ml) and the combined extracts washed twice with water (2×50 ml), dried (Na2SO4), and evaporated to afford the title product as a pale yellow oil (12.5 g) which was used without further purification. 1H NMR (CDCl3) δ: 1.7-2.0 (6H, m), 2.15-2.3 (2H, m), 3.3 (6H, s). Mass Spectrum (Electrospray LC/MS): Found 112 (MH+−HCN). C8H14N2 requires 138.
後処理
- temperaturecooled (ice bath)
- customthe crude reaction mixture
- extractionwas extracted three times with diethyl ether (3×200 ml)
- washthe combined extracts washed twice with water (2×50 ml)
- dry with materialdried (Na2SO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-8614649301fe4c808a29ae62cc1fd84c
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745642B2
反応ノート
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