谢谢大家。
我已经查到文献了,
和大家分享一下吧。
In a dry 3-l. flask, fitted with a mercury-sealed stirrer, a 500-cc. dropping funnel, and a condenser provided at its upper end with a drying tube containing a mixture of calcium chloride and soda-lime (Note 1), is placed 48.6 g. (2 atoms) of magnesium turnings. There are then added 200 cc. of dry ether, a small crystal of iodine, and about 25 cc. of a solution of 253 g. (230 cc., 2 moles) of freshly distilled benzyl chloride in 1 l. of dry ether. If the reaction does not start at once, the flask is partially immersed in a bath containing water heated to about 40°. As soon as the ether begins to boil, and reaction sets in, the bath is removed and stirring is commenced. The remainder of the benzyl chloride in ether can be added during the course of one-half hour if the reaction is regulated by cooling the greater part of the flask by immersion in ice water (Note 2). The reaction will continue for about fifteen minutes after all the benzyl chloride has been added, and then the mixture is refluxed gently for about fifteen minutes.
主要就是注意无水无氧。
把盐酸处理过后干燥的镁屑装入三口瓶中,接上滴液漏斗,回流冷凝管,密封后无水无氧处理。
用少量THF把镁覆盖,然后滴加苄溴。
反应引发后,用干的THF逐渐稀释滴液漏斗中的苄溴。
滴完后,加热微沸回流2小时左右就可以了。
最后最好滴定其浓度。
苄基格氏试剂和一般的格氏试剂不一样,特别容易自很偶联,
温度要控制得很低才行
但是具体操作我还是不知道,,
这个东西不能四氢呋喃回流的,太容易耦联了
溶剂用甲基四氢呋喃,可以有效防止自身偶联。
谢谢大家。
我已经查到文献了,
和大家分享一下吧。
In a dry 3-l. flask, fitted with a mercury-sealed stirrer, a 500-cc. dropping funnel, and a condenser provided at its upper end with a drying tube containing a mixture of calcium chloride and soda-lime (Note 1), is placed 48.6 g. (2 atoms) of magnesium turnings. There are then added 200 cc. of dry ether, a small crystal of iodine, and about 25 cc. of a solution of 253 g. (230 cc., 2 moles) of freshly distilled benzyl chloride in 1 l. of dry ether. If the reaction does not start at once, the flask is partially immersed in a bath containing water heated to about 40°. As soon as the ether begins to boil, and reaction sets in, the bath is removed and stirring is commenced. The remainder of the benzyl chloride in ether can be added during the course of one-half hour if the reaction is regulated by cooling the greater part of the flask by immersion in ice water (Note 2). The reaction will continue for about fifteen minutes after all the benzyl chloride has been added, and then the mixture is refluxed gently for about fifteen minutes.
Org. Syn. Coll. Vol. I, 1941, 471,
其实,大家都知道做敏感的格式用乙醚比较好,但是考虑到安全及放大,一般不用乙醚做溶剂。