铜粉

到 查阅并下载Collective Volume 3, page 339 ，用碘的丙酮溶液活化（见下文）

1. Ordinary copper bronze does not always give satisfactory results in the Ullmann reaction. More

uniform results are obtained if the copper bronze is prepared as suggested by Kleiderer and Adams.1

The copper bronze is treated with 2 l. of a 2% solution of iodine in acetone for 5–10 minutes. The

product is then collected on a Büchner funnel, removed, washed by stirring into a slurry with 1 l. of a

1:1 solution of concentrated hydrochloric acid in acetone, and again filtered. The copper iodide

dissolves, and the copper bronze remaining is separated by filtration and washed with acetone. It is then

dried in a vacuum desiccator. It should be used immediately.

Synthesis and Reactivity in Inorganic and Metal-Organic Chemistry Volume 3,

Issue 4, 1973 选择语言▼ Translator disclaimer

Synthesis of Phosphonium Salts of Mixed

Chloro-Bromo Metallate Complexes 1

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DOI:

10.1080/00945717308057280

John L. Burmeister a , Joel L. Silver a , Edward T. Weleski Jr.a , Edward E. Schweizer a & Charles M. Kopay a

pages 339-358

Publishing models and article dates explained

∙Received: 3 Apr 1973

∙Accepted: 24 May 1973

∙Published online: 06 Dec 2006

Synthesis of phosphonium salts of mixed chloro-bromo metallate complexes [求助]Over syntheses in the diphenyl line. [machine translation]和

Synthesis in the bip

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作者:

Ullmann, F

文题:

1. Over syntheses in the diphenyl line. [machine translation]和

2. Synthesis in the biphenyl series. I

期刊名:

Berichte der Deutschen Chemischen Gesellschaft

期刊年份:

1901

卷(期),起止页码:

34，2174-2185和34，478-480

全文链接:

https:///scifinder/view/scifinder/scifinderExplore.jsf

Org.Synth,1943,Coll.Vol.2;446

[Machine Translation of Descriptors]. By heating up aromatic halogen nitro compounds with copper powder ("copper bronze", see Ber. German Chem. Society 29. 1878; C. 96. II. 533) one receives easy and smooth diphenyl derivative; the reaction occurs also then, if the nitro group does not stand for the halogen is, however, in this case limited to the iodine nitro compounds. At all iodine lets itself take out through copper particularly easily, because the analogous conversion took place also with the iodine benzene, -toluene, -naphthalene, among others. The reaction volume-pulls itself at temperatures of for instance 180-260°; bodies also easily mobile halogen atoms must the vehemence of the effect by diluting with nitrobenzene or causing sand be moderated. Of TAEUBER (Ber. German. Chem. Society 24. 197) 2.2'-dinitrodipheyl already described, NO2. C6H4. C6H4. NO2, formed to 76%, as 5 g whether Rome nitrobenzene in the sulfuric acid bat h on 200° for the theory, warmed up and then 3 g copper-bronze in small helpings under steady accomplish of the mass with the thermometer registered became. For the preparation in larger scales became 30 g o-chloronitrobenzene with 50 g sand on 200-210° he ated up and then 30 g copper so slowly registered that the temperature 250° did not exceed (above 260° decomposing itself the melt lower partial formation of carbazoles); finally still 1/2 hour on 240-245° became heated up and the product then with alcohol or benzene extracts. M-chlorine and m-Bromnitrobenzene were copper not changed by, m-Iodinenitrobenzene (boiling point 278°) supplied with 220-225°, on the other hand easily 3.3' - dinitrodiphenyl, C12H8O4N2; yellow, star shaped grouped needles from tolue ne; melting point 200°; easily soluble into warm benzene, glacial acetic acid; more with difficulty soluble in alcohol (see BRUNNER, WITT, Ber. German. Chem. Ges. 20. 1028). 4.4'-Dinitrodiphenyl, C12H8O4N2, from p-iodine nitrobenzene [KP726, 287° (correcte d)] and copper with 220-235° obtained; yellow needles from toluene; melting point 237° (FITTIG: 233°); few soluble in alcohol; somewhat more easily soluble in benzene. 2.2', 4.4' - tetranitrodiphenyl, (NO2) 2C6H3. C8H5. (NO2) 2, formed by one-hour cooking of 4-Chlor or 4-Brom-l, 3-dinitrobenzol with copper in nitrobenzene; also, as 10 g diphenyls developed in 60 g of nitric acid lower water cooling registered and the red solution, from which crystals of 4-Nitrodiphenyl separated, with weak fuming sulfuric acid (3-4% SO3) were shifted. Yellowish prisms from benzene; melting point 163°; few soluble in alcohol, ether; easily soluble into hot glacial acetic acid, benzene. By registering 10 g m-iodine nitrobenzene in 40 g of nitric acid of the density 1.5 and causing concentrated sulfuric acid, until the liquid became yellow, one receives within 24 hours of 4-Jod-1.2-dinitrobenzol, (NO2) 2C6H3I; yellow crystals from alcohol; melting point 74.5°. Reacted, contrary to analogous chlorine and bromine compound, with co pper with 230 to 250° under formation of 3.3', 4.4'-Tetranitrodiphenyl, C12H8N4; yellow prisms from alcohol; melting