當前位置:律師網大全 - 專利查詢 - 苯乙腈乙酸乙脂甲醇鈉反應二小時ph也調了也過濾了靜止幾小時,怎麽還是壹杯水什麽物體也沒有。哪裏做了

苯乙腈乙酸乙脂甲醇鈉反應二小時ph也調了也過濾了靜止幾小時,怎麽還是壹杯水什麽物體也沒有。哪裏做了

這個反應是需要加熱的,而且醇鈉的質量要保證。下邊是壹個專利的操作,不同之處是使用了現場制備的乙醇鈉,妳可以參考壹下。

25 g (0.213 mol) portion of phenylacetonitrile and 33 ml of ethyl acetate were added to an ethanol solution of sodium ethoxide prepared from ethanol (150 ml) and 6.38 g (0.277 mol) of metallic sodium and then heated under reflux for 3 hours. After cooling, this was concentrated under a reduced pressure, and the thus obtained residue was mixed with water and dichloromethane to separate the organic layer. This was washed with 1 N hydrochloric acid and brine and dried over magnesium sulfate, and then the solvent was evaporated. The thus obtained residue was applied to a silica gel column chromatography to obtain 3.15 g (9percent) of the title compound as a colorless oily substance from a n-hexane-ethyl acetate (5:1-->3:1 v/v) eluate. MS (FAB)m/z: 160 (M+1)+. 1H-NMR (CDCl3)δ: 2.27 (3H, s), 4.68 (1H, s), 7.36-7.52 (5H, m).

  • 上一篇:專利去哪申請?有代理公司嗎?
  • 下一篇:專利申請可以委托機構代辦嗎
  • copyright 2024律師網大全