Sulphuryl chloride preparation

A wide range of chlorine-containing oxidants have been used for the preparation of sulphones from sulphoxides. These reagents include chlorine, hypochlorites, sulphuryl chloride and IV-chloro compounds. 

Preparation of Sulphuryl Chloride. Before performing this synthesis, dry activated carbon in a vacuum (10- mmHg) in a test tube and heat it during 40-50 min with the flame of a burner. 

This substance was prepared by Franchimont [69] from dimethylsulphamide obtained by the interaction of methylamine and sulphuryl chloride ... 

Herz [72] described the preparation of this substance by the action of ethanolamine on sulphuryl chloride, followed by the nitration of the dihydroxyethylsulphamide so obtained. 

Sulphuryl Chloride, S02C12.—As would be expected, it is possible to obtain an acid chloride, S02C12, corresponding with sulphuric acid, SO2(OH)2, but the chloride cannot be prepared by the action of phosphorus pentachloride on sulphuric acid or sulphur trioxide, these reagents yielding pyrosulphuryl chloride.7... 

Formation and Preparation.—Chlorine and sulphur dioxide will only unite under some accelerating influence. It was by the interaction of these gases in sunlight that sulphuryl chloride was first obtained by Regnault in 183S. 

A convenient method for the laboratory preparation of sulphuryl chloride consists in boiling chlorosulphonic acid with about one per cent, of mercury or mercuric sulphate under a reflux condenser kept at a temperature of 70° C. in order to return to the flask any unchanged chlorosulphonic acid ... 

The following methods are available for the preparation of chloro-sulphonic acid (1) The substance can be obtained by the gradual action of moisture (e.g. atmospheric moisture) on sulphuryl chloride a similar reaction occurs with sulphuric acid and is more easily regulated ... 

Another method of preparation for pure sulphamide is to dissolve the product of the reaction between sulphuryl chloride and liquid ammonia in a small quantity of water and acidify the solution in order to cause hydrolysis. After two or three days, when hydrolysis is complete, the mixture is evaporated to dryness in vacuo and the residue extracted with ethyl acetate. The sulphamide is dissolved out and on evaporating off the ethyl acetate, pure sulphamide is obtained.3... 

The technical product frequently contains traces of acids, sulphur chlorides and sulphuryl chloride it is essential to remove these before using the reagent for the preparation of acid chlorides, etc. Commercial purified thionyl chloride is satisfactory for most purposes. A colourless product of high purity may be obtained by either of the following methods. 

In the chemical industry chlorine is used for the production of various chemical compounds, such as hydrochloric acid, hypochlorites, chlorates, bleaching powder, aluminium chloride, corrosive sublimate, cupric chloride, carbon tetrachloride, tin recovery from used cans, sulphuryl chloride, for extraction of bromine from Stassfurt waste liquors, etc. In the organic chemical industry it is used for the chlorination of aliphatic and cyclic organic compounds, for the preparation of medicaments, the manufacture of plastics, insecticides, fungicides and herbicides. Monochloracetic acid, ethylene chlorhydrine, chloral, chlor-... 

Phosphorus may also be combined to form the trichloride by passing its vapour over mercurous or mercuric chloride3 or cupric chloride,5 or by passing the vapour of sulphur monochloride over phosphorus,6 or by heating red phosphorus with sulphuryl chloride.7 It is possible to prepare it directly from calcium phosphate by heating this with silica and charcoal and passing over it the vapour of sulphur monochloride —... 

Sulphuryl chloride was chiefly prepared during the war for the manufacture of methyl and ethyl chlorosulphonates, but was occasionally employed also in admixture with cyanogen chloride, phosgene or chloropicrin (Prentiss). 

The usual method of preparing this war gas is by the action of methyl alcohol on sulphuryl chloride ... 

Synthesis of Phosphoric Acids and their Derivatives.-New approaches to the preparation of dialkyl phosphorofluoridates include the treatment of a vinyl phosphate, e.g.,(l), or an irninophosphace, e.g.,(2), with triethylamine tris(hydrogen fluoride) when the alkyl group consists of a suitably protected nucleoside, the reaction between mono(crimethylsilyl) phosphite in pyridine and sulphuryl chloride fluoride at -30° has been successfully explored. Dibenzyl phosphorofluorldate, hitherto unreported, has been obtained from tecrabenzyl diphosphate and caesium fluoride, and also from the reaction between dibenzyl hydrogen phosphate and 2-fluoro-N-methylpyridinlum tosylate. ... 

The thieten 1,1-dioxide (48) has been prepared by cycloaddition of an enamine and sulphene at 0°C. Mild thermolysis causes a ready retrocyclo-addition to occur. Additional stable 3-sultines have been isolated, by the reaction of the anion of a sulphoxide with a ketone and cyclization of the resulting j3-hydroxy-sulphoxide with sulphuryl chloride. Treatment of 2-methylthietan (49) with alumina at 150-350 °C results in the formation of tetrahydrothiophen and but-3-enethiol. ... 

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