苯乙腈乙酸乙脂甲醇钠反应二小时ph也调了也过滤了静止几小时,怎么还是一杯水什么物体也没有.哪里做了,在什么步骤后才结晶.
来源:学生作业帮助网 编辑:作业帮 时间:2024/07/05 12:31:19
![苯乙腈乙酸乙脂甲醇钠反应二小时ph也调了也过滤了静止几小时,怎么还是一杯水什么物体也没有.哪里做了,在什么步骤后才结晶.](/uploads/image/z/2222746-34-6.jpg?t=%E8%8B%AF%E4%B9%99%E8%85%88%E4%B9%99%E9%85%B8%E4%B9%99%E8%84%82%E7%94%B2%E9%86%87%E9%92%A0%E5%8F%8D%E5%BA%94%E4%BA%8C%E5%B0%8F%E6%97%B6ph%E4%B9%9F%E8%B0%83%E4%BA%86%E4%B9%9F%E8%BF%87%E6%BB%A4%E4%BA%86%E9%9D%99%E6%AD%A2%E5%87%A0%E5%B0%8F%E6%97%B6%2C%E6%80%8E%E4%B9%88%E8%BF%98%E6%98%AF%E4%B8%80%E6%9D%AF%E6%B0%B4%E4%BB%80%E4%B9%88%E7%89%A9%E4%BD%93%E4%B9%9F%E6%B2%A1%E6%9C%89.%E5%93%AA%E9%87%8C%E5%81%9A%E4%BA%86%2C%E5%9C%A8%E4%BB%80%E4%B9%88%E6%AD%A5%E9%AA%A4%E5%90%8E%E6%89%8D%E7%BB%93%E6%99%B6.)
苯乙腈乙酸乙脂甲醇钠反应二小时ph也调了也过滤了静止几小时,怎么还是一杯水什么物体也没有.哪里做了,在什么步骤后才结晶.
苯乙腈乙酸乙脂甲醇钠反应二小时ph也调了也过滤了静止几小时,怎么还是一杯水什么物体也没有.哪里做了,在什么步骤后才结晶.
苯乙腈乙酸乙脂甲醇钠反应二小时ph也调了也过滤了静止几小时,怎么还是一杯水什么物体也没有.哪里做了,在什么步骤后才结晶.
这个反应是需要加热的,而且醇钠的质量要保证.下边是一个专利的操作,不同之处是使用了现场制备的乙醇钠,
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).