Iron powder obtained

Morphological characteristics. Iron powders obtained by the two-steps procedure described earlier are formed of polyhedral, and even often cubic, nonagglomerated particles with a rather narrow size distribution and a mean size in the... 

The antiparasitic drug clorsulon (206), contains a rather unusual trichloroethylene group. This function is established early in the syntliesis by treatment of the perhalogenated compound 203 obtained from reduction of 202 with iron powder. Chlorosulfonation of 204 by means of chloro-sulfonic acid, followed by conver.sion of. sulfonyl chloride 205 to the amide, gives clorsulon (206) 153],... 

The ethyl acetate solution is then washed with water, dried and evaporated. To remove any selenium still present, the residue is dissolved in 200 cc of methanol and mixed with 100 g of iron powder and 2 g of active carbon. The mixture is heated for 30 minutes with stirring under reflux, then filtered with suction, washed with methanol and the solution evaporated in vacuo. The residue is then chromatographed on 900 g of aluminum oxide. The residues of the evaporated benzene and ether fractions are treated with active carbon in methanol or acetone, evaporated again, and the residue recrystallized from a mixture of acetone and ether. There are obtained 17.5 g of pure 1-dehydro-17a-methyl-testosterone which melts at 163° to 164°C. 

When thionyl chloride is used, diaryl sulfoxides are usually the main products. Unsymmetrical diaryl sulfides can be obtained by treatment of an aromatic compound with an aryl sulfenyl chloride (ArSCl) in the presence of a trace amount of iron powder.Aromatic amines and phenols can be alkylthiolated (giving mostly ortho product) by treatment with an alkyl disulfide and a Lewis acid catalyst. With certain substrates (primary amines with a chloro group, or a group not replaceable by chloro, in the para position), treatment with S2CI2 and NaOH gives thiophenolate salts ... 

Pyron A process for making iron powder by reducing mill-scale, obtained from steelworks, with hydrogen. In operation in the United States in places where cheap hydrogen is available near steelworks. 

Mix 0.25M substituted benzaldehyde, 0.3M nitroethane, 50 ml dry toluene and 5 ml n-butylamine (or other amine), and reflux 3 hours with a Dean-Stark trap (or prepare the nitro-propene as described elsewhere here). Add 50 g iron powder and 1 g FeCl3 optional) and reflux while adding 90 ml concentrated HCI over 3 hours. Reflux 1 hour more, add 2 liters of water and extract 3 times with ether, then dry and evaporate in vacuum (or steam distill until about 3.5 liters of distillate is obtained extract the distillate 3 times with toluene wash the toluene layers with 7 g NaHS03 in 225 ml of water, then 3 times with water and dry, evaporate in vacuum) to get the ketone. Mix 0.13M ketone, 28 g formamide (or dimethyl-formamide if the N.N-dimethylamine is desired) and 3 ml formic acid and heat at 160°. Add 3 more ml formic acid and heat 16 hours at 170-180° adding formic acid from time to time to keep the pH acid. Distill off the water formed (about 16 ml), cool and extract with 3X70 ml benzene. Distill off the benzene and reflux the residue 7 hours with 30 ml concentrated HCI. Chill, basify with 10% NaOH and extract with 3X70 ml ether. Dry and evaporate the ether in... 

Metallic iron is used in the analytical laboratory in the form of thin, polished wire (piano wire), or gray powder obtained by reduction with hydrogen (iron by hydrogen), and also in the form of the ordinary gray, lustrous powdered iron. 

The iron used may be either iron powder or iron filings, but it should pass a 100-mesh sieve in order to give invariable results. If iron particles of larger size are used, the reduction may be incomplete although complete reduction was obtained with a sample of iron powder contaminated with filings. 

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