反应详情

温度

150 °C

This product was prepared by a modification of the general procedure described in Shimizu, T. et al. Bull.Chem.Soc.Jpn. 1985, 58, 2519. A mixture of 4-chlorobenzonitrile (1.7 g, 12.2 mmol), and diethyl nitromalonate (2.5 g, 12.2 mmol) in dodecane (20 mL) was heated at 150° C. for 15 h. After the reaction was complete, the mixture was allowed to cool to room temperature and was then concentrated in vacuo. The residue was purified by flash chromatography to yield ethyl 5-(4-chlorophenyl)-1,2,4-oxadiazole-3-carboxylate as a light brown solid: mp 88°-89° C.; 1H NMR (300 MHz, CDCl3) δ (TMS) 8.15 (dt, Jt =2.3, Jd =8.7, 2H, arom), 7.54 (dt, Jt =2.3, Jd =8.7, 2H, arom), 4.55 (q, J=7.1, 2H, OCH2), 1.47 (t, J=7.1, 3H, OCH2CH3).

1. customThis product was prepared by a modification of the general procedure
2. temperatureto cool to room temperature
3. concentrationwas then concentrated in vacuo
4. customThe residue was purified by flash chromatography