Ethylene Glycol → (2-Ethyl-[1,3]dioxolan-2-yl)-acetonitrile
반응식
[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]참가 물질
6
실험 절차
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)
후처리
- washwashed with saturated sodium bicarbonate solution
- dry with materialThe organic phase is dried over MgSO4
- filtrationfiltered
- customthe solvent evaporated
출처 및 근거
- ORD 기록
- ord-2a163798fe114771b0fd8b5b19b1ff9a
- 출처 데이터셋
- uspto-grants-2007_10
- 특허 번호
- US07288537B2
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