定制各类格氏试剂

问题:奥拉试剂 是什么东东啊
类型:交流
提问:hsc
等级:
版块:氟化学(maurice,)
信誉:100%
回复:3
阅读:1556
时间:2006-08-24 09:26:50  编辑    加入/取消收藏    订制/取消短消息    举报该贴    

各位
奥拉试剂 谁能介绍点具体的么 
回复人:yfzhang, (高级工程师团队,为氟化学化工创业者助一臂之力) 时间:2006-08-25 12:04:35   编辑 1楼
奥拉试剂不是东东,是东西!
奥拉试剂是无水氟化氢与三级胺(如三乙胺,三丁胺,吡啶等)的复合物。一个三级胺分子能与几个氟化氢分子结合,结合后,氟化氢混合物的沸点升高,使一些用氟化氢的反应可在常压下进行。因为这个试剂首先是化学家奥拉发现的,因此叫奥拉试剂。

化学创新无极限,你也可搞一个HSC什么什么的,只要你将把艰苦的化学工作进行到底!

[该帖子已被yfzhang在2006-8-26 1:54:03编辑过]


回复人:hsc, (交流,交流,学习,学习!~~~~~锂电池 电解液 药物合成) 时间:2006-08-31 08:49:47   编辑 2楼
Thank you !!!


回复人:yfzhang, (高级工程师团队,为氟化学化工创业者助一臂之力) 时间:2006-09-08 09:20:23   编辑 3楼
请hsc下载阅读!

Organic Syntheses, Coll. Vol. 6, p.628 (1988); Vol. 58, p.75 (1978).
FLUORINATIONS WITH PYRIDINIUM POLYHYDROGEN FLUORIDE REAGENT: 1-FLUOROADAMANTANE
[Tricyclo[3.3.1.13,7]decane, 1-fluoro-]


Submitted by George A. Olah1 and Michael Watkins.
Checked by Paul G. Williard and G. Büchi.
1. Procedure
Caution! Proper precautions must be used when handling anhydrous hydrogen fluoride and pyridinium polyhydrogen fluoride. Hydrogen fluoride is extremely corrosive to human tissue, contact resulting in painful, slow-healing burns. Laboratory work with HF should be conducted only in an efficient hood, with the operator wearing a full-face shield and protective clothing (Note 1).
A. Pyridinium polyhydrogen fluoride (1). A tared, 250-ml., polyolefin bottle is equipped with a polyolefin gas-inlet and drying tube inserted through holes in the cap and sealed with Teflon tape. The bottle is charged with 37.5 g. (0.475 mole) of pyridine (Note 2) and cooled in an acetone–dry ice bath. After the pyridine has solidified, 87.5 g. (4.37 moles) of anhydrous hydrogen fluoride (Note 3) is condensed from a cylinder into the bottle through the inlet tube. The amount of hydrogen fluoride is determined by weighing the bottle. After the hydrogen fluoride has cooled, the bottle is cautiously swirled with cooling until the solid dissolves (Note 4). The solution can now be safely allowed to warm to room temperature.
B. 1-Fluoroadamantane (2). A 250-ml., polyolefin bottle is equipped with a Teflon-coated magnetic stirring bar and a polyolefin drying tube inserted through a hole in the cap and sealed with Teflon tape. The bottle is charged with 5.0 g. (0.033 mole) of 1-adamantanol (Note 5) and 50 ml. of pyridinium polyhydrogen fluoride (1). The solution is allowed to stir for 3 hours at ambient temperature, after which 150 ml. of petroleum ether is added, and stirring is continued for another 15 minutes. The resulting two-phase solution is transferred to a 250-ml., polyolefin separatory funnel, and the bottom layer is discarded (Note 6). The organic layer is washed successively with 50 ml. of water, 50 ml. of a saturated sodium hydrogen carbonate solution and 50 ml. of water, then dried over magnesium sulfate. After the organic layer is filtered, the solvent is removed under reduced pressure (Note 7), yielding 4.5–4.6 g. (88–90%) of adamantane 2 as a white powder, m.p. 225–227° (sublimes in a sealed capillary) (Note 8), which can be purified by vacuum sublimation or by recrystallization from methanol-carbon tetrachloride.
2. Notes
1. The recommended first-aid for a hydrogen fluoride burn is to flood with water, pack with ice, and get medical attention as quickly as possible. Local medical personnel should be alerted and prepared when work with hydrogen fluoride is planned. Directions for proper medical treatment2 are given in Org. Synth., Coll. Vol. 5, 66 (1973).
2. The submitters used A.C.S. certified reagent grade pyridine from Fisher Scientific Company which was distilled from potassium hydroxide prior to use.
3. The submitters obtained anhydrous hydrogen fluoride from Harshaw Chemical Company, and the checkers purchased this reagent from Matheson Gas Products.
4. The dissolution is an extremely exothermic process that can be violent if the bath temperature is not carefully controlled at −78°. A preferred procedure developed by Dr. A. E. Feiring, Central Research and Development Department, Du Pont Experimental Station, involves keeping the pyridine as cold as possible without freezing (ca. −40°), then slowly condensing the hydrogen fluoride into the vessel so that the entire mixture remains liquid during the preparation. Stirring is also helpful.
5. This was obtained from Aldrich Chemical Company, Inc., and used without further purification.
6. The inorganic layer can be safely disposed by slow addition to large amounts of ice-cold water.
7. Since 1-fluoroadamantane sublimes easily, the water bath should be controlled at about 32°, and the vacuum evaporation of the solvent limited to as short a time as possible.
8. GC and IR analysis indicate no detectable amount of starting alcohol. 1H NMR of adamantane 2 (CDCl3) yields a series of multiplets centered at δ 1.62, 1.86, and 2.18.
3. Discussion
1-Fluoroadamantane can also be prepared by halogen exchange of the bromide with silver fluoride3 or zinc fluoride.4 The procedure described is more convenient and economical than the halogen exchanges, and has found successful application in the preparation of a wide variety of secondary and tertiary fluorides from the corresponding alcohols, with yields generally within the range of 70–90%5 (Table I).


References and Notes
Hydrocarbon Research Institute, Department of Chemistry, University of Southern California, Los Angeles, California 90007.
C. M. Sharts and W. A. Sheppard, Org. React., 21, 192, 220–223 (1974).
R. C. Fort and P. v. R. Schleyer, J. Org. Chem., 30, 789 (1965).
K. S. Bhandari and R. E. Pincock, Synthesis, 655 (1977).
G. A. Olah, M. Nojima, and I. Kerekes, Synthesis, 786 (1973).
W. J. Middleton and E. M. Bingham, Org. Synth., Coll. Vol. 6, 440, 835 (1988).
G. A. Olah, M. Nojima, and I. Kerekes, Synthesis, 779 (1973).
G. A. Olah and J. Welch, Synthesis, 896 (1974).
G. A. Olah, M. Nojima, and I. Kerekes, Synthesis, 780 (1973).
G. A. Olah and J. Welch, Synthesis, 654 (1974).
G. A. Olah and J. Welch, Synthesis, 652 (1974).
S. Matsuura, C. H. Niu, and J. S. Cohen, J. Chem. Soc. Chem. Commun., 451 (1976).




问题讨论没有结束...
您尚未进入本论坛,登录之后才可以回贴
用户名:密码:    游客  新用户免费注册
7msec



版权所有 中国化学化工论坛 
可转载本站文章 但请务必注明出处 本站法律顾问 方利律师  
www.ccebbs.com E-Mail:ccebbs00@126.com
Chinese Chemistry and Chemical Engineering BBS