DICYCLOPENTADIENYLIRON

DICYCLOPENTADIENYLIRON
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DOI:
10.1039/jr9520000632
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发表时间:
1952-01-01
期刊:
JOURNAL OF THE CHEMICAL SOCIETY
影响因子:
--
通讯作者:
TREMAINE, JF
TREMAINE, JF
中科院分区:
其他
文献类型:
--
作者:
MILLER, SA;TEBBOTH, JA;TREMAINE, JF

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还原铁(在氧化铝和氧化钾存在下,优选氧化钼存在下)与环戊二烯在氮气中在300”下反应,得到2黄色化合物C1 H1 Fe,m. p.172 -5-173”,认为是二环己基铁。它在100”以上升华而不分解,在蒸汽中挥发,可溶于有机溶剂。该化合物的形成仅进行10-15分钟,之后,仅在铁的小心氧化和再还原之后进行进一步的反应。在玻璃管中于250”的氮气中加热后,通常在首次制备时,铁化合物含有少量吸附的氮,这些氮被充分牢固地保持,从而给出氮的正钠熔试验。迄今为止,还没有人描述过只含有碳、氢和铁的化合物,而且用铁直接取代碳上的氢也是不可行的。现在已经发现,可以使还原铁以公知的”双促进合成氨催化剂”的形式与环己基氨反应。
Reduced iron (in presence of alumina and potassium oxide, and preferably also molybdenum oxide) reacts with cyclopentadiene in nitrogen at 300" to give 2 yellow compound C,, H,, Fe, m. p. 172-5-173", believed to be dicyclopentadienyliron. It sublimes above 100" without decomposition, is volatile in steam, and soluble in organic solvents. The formation of this compound proceeds only for 10-15 minutes, after which further reaction is only effected after careful oxidation and re-reduction of the iron. After being heated in a glass tube at 250" in nitrogen, and frequently as first prepared, the iron compound contains small amounts of adsorbed nitrogen which is sufficiently firmly held to give positive sodium-fusion tests for nitrogen. It has not been possible to use this property to make the material behave as a catalyst for ammonia formation.COMPOUNDS containing only carbon, hydrogen, and iron have not hitherto been described, and the direct replacement of hydrogen attached to carbon by iron would not be expected to be feasible. It has now been found that reduced iron, in the form of the well-known" doubly-promoted synthetic ammonia catalyst," can be made to react with cyclo-