Iron chlorides dehydration

Available forms (2) Powdered iron. Derived (a) by treatment of ore or scrap with hydrochloric acid to give ferrous chloride solution, which is then purified by filtration, vacuum crystallized, and dehydrated to ferrous chloride dehydrate powder this is reduced at 800C to metallic iron (briquettes or powder) of 99.5% purity (b) by thermal decomposition of iron carbonyl [Fe(C05)] at 250C (99.6-99.9% pure) (c) by hydrogen reduction of high-purity ferric oxide or... 

The dehydration of moist inorganic salts with water of crystallization content is, in general, a complex task. The loss of crystalline water usually consists of several components with different temperature or residence time requirements for each case. In the course of dehydration, the material to be processed (e.g., ZnCl2 or MnCy may form undesirable compounds. In numerous cases, as with magnesium chloride and iron chloride, oxygen impedes the full loss of crystal water as a result of heat effects. On the basis of these problems, publications dealing with successful dehydration experiments conducted in spouted bed equipment are of particular interest. 

Uses of hydrogen chloride—Hydrogen chloride is sometimes used in the preparation of an ester, for example ethyl benzoate, where it acts as both an acid catalyst and a dehydrating agent. Hydrochloric acid is used primarily to produce chlorides, for example ammonium chloride. It is extensively used in the manufacture of anilme dyes, and for cleaning iron before galvanising and tin-plating. 

Ironilll) chloride is a black, essentially covalent solid, in which each iron atom is surrounded octahedrally by six chlorine atoms. It is prepared by direct combination of iron with chlorine or by dehydration of the hydrated chloride, by one of the methods given on p.343). 

Benzyl acetate was prepared by addition of benzyl chloride (containing 0.6% pyridine as stabiliser) to preformed sodium acetate at 70°, followed by heating at 115°, then finally up to 135°C to complete the reaction. On one occasion, gas began to be evolved at the end of the dehydration phase, and the reaction accelerated to a violent explosion, rupturing the 25 mm thick cast iron vessel. This was attributed to presence of insufficient pyridine to maintain basicity, dissolution of iron by the... 

Bis(perfluoroalkyl)-l,3,4-oxadiazoles (285) are attacked readily by hydrazine with ring opening and formation of the perfluoroacylated hydrazidines (286). Concurrent dehydration and oxidation of these intermediates with iron(III) chloride produces the corresponding 3,6-bis(perfluoroalkyl)-l,2,4,5-tetrazines (287). Ring closure of (286) without oxidation produces the corresponding 3,5-bis(perfluoroalkyl)-4-amino-l,2,4-triazoles (66JOC781). 

Mischmetal is produced commercially by electrolysis, The usual starting ingredient is the dehydrated rare earth chloride produced from monazite or bastnasite. The mixed rare earth chloride is fused in an iron, graphite, or ceramic crucible with the aid of electrolyte mixtures made up of potassium, barium, sodium, or calcium chlorides. Carbon anodes are immersed in the molten salt. As direct current flows through the cell, molten mischmetal huilcls up in the bottom of the crucible. This method is also used to prepare lanthanum and cerium metals. 

Anhydrous iron(II) chloride has been prepared by passing hydrogen chloride over iron, by reducing iron(III) chloride with hydrogen, and by dehydrating one of the hydrates of iron(II) chloride. A new procedure is outlined here.1,2... 

By treatment of the adduct with ethylmagnesium bromide and iron(m) chloride followed by acid. By acylation and ozonolysis. In the presence of lithium t-butoxide with diisopropylmagnesium alone, substantial amounts of reduction are observed. rfBy dehydration of the alcohol. "Reaction at -50° reaction in refluxing ether gave only 5%. Reaction in toluene containing 5% THF. 

The chemistry of iron vinylidene complexes is dominated by the electrophilicity of the carbon atom adjacent to the iron organometallic unit. While addition of water leads to an acyl complex (i.e., the reverse of the dehydration shown in equation 10), addition of an alcohol leads to a vinyl ether complex. Similarly, other iron vinyl complexes can be prepared by the addition of thiolate, hydride, or an organocuprate (Scheme 33). " The nucleophilic addition of imines gave enaminoiron intermediates that could be further elaborated into cyclic aminocarbenes. This methodology has been used to provide access to /3-lactams and ultimately penicillin analogs, and good diastereoselectivities were observed (6 1-15 1) (Scheme 34). 04 Iso, vinylidene complexes are intermediates in cyclizations of alkynyl irons with substituted ketenes, acid chlorides, and related electrophiles an example is shown (equation 11). These cyclizations led to the formation of a series of isolable and characterizable cyclic vinyl iron complexes. 

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