Ethylene Glycol → (2-Ethyl-[1,3]dioxolan-2-yl)-acetonitrile
反応式
[O:1]=[C:2]([CH2:6][CH3:7])[CH2:3][C:4]#[N:5].[CH2:8](O)[CH2:9][OH:10].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1.C(OCC)(=O)C>[CH2:6]([C:2]1([CH2:3][C:4]#[N:5])[O:10][CH2:9][CH2:8][O:1]1)[CH3:7]参加物
6
実験手順
A solution of 3-oxo-pentanenitrile (1.582 g, 16.49 mmol), ethylene glycol (1.026 ml, 84.59 mmol) and a catalytic amount of p-Toluene Sulphonic acid (8 mg) in Toluene (10 ml) is refluxed at 150° C. for 2 days using Dean-Stark apparatus. The reaction mixture is diluted with ethyl acetate and washed with saturated sodium bicarbonate solution. The organic phase is dried over MgSO4, filtered, and the solvent evaporated to yield (2-ethyl-[1,3]dioxolan-2-yl)-acetonitrile. 1H NMR (400 MHz, CDCl3) d 4.15(2H,m), 4.05 (2H, m), 2.65 (2H, s), 1.80 (2H, q), 0.95 (3H, t)
後処理
- washwashed with saturated sodium bicarbonate solution
- dry with materialThe organic phase is dried over MgSO4
- filtrationfiltered
- customthe solvent evaporated
出典と根拠
- ORDレコード
- ord-2a163798fe114771b0fd8b5b19b1ff9a
- 出典データセット
- uspto-grants-2007_10
- 特許番号
- US07288537B2
反応ノート
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