Preparation of Sulphuryl Chloride

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. 

Put the dried activated carbon loosely on a glass wool substrate into each of the bulbs of a cooler on standard ground glass joints (the number of bulbs should be at least six). The carbon should occupy at most one-half of the volume of a bulb. Camphor may be used instead of the activated carbon. 

Assemble an apparatus as shown in Fig. 71. Connect cooler 4 to a 100-ml round-bottomed flask with the aid of special adapter 1. Connect apparatuses for preparing dry chlorine (see Fig. 61) and 

To purify the sulphuryl chloride, connect the receiver flask to an apparatus for distillation under atmospheric pressure provided with a dephlegmator (see Fig. 70). Heat the flask in a water bath and distil the substance, collecting the fraction that boils at 68-70 °C. 

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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 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. 

These were synthesized by the reaction of sulphuryl chloride with dialkylcyanoamides. The sulphamoyl guanidines (308) can also be prepared by the reaction of 307 with trimethylsilylamines307 (equation 100). 

In the technical preparation of acetyl chloride sulphuryl chloride, SO2CI2, is used instead of the chlorides of phosphorus, on account of the cheapness of the sulphur compound. Acetyl chloride is prepared by passing a mixture of chlorine and sulphur dioxide over anhydrous sodium acetate. In the presence of the salt sulphuryl chloride is first formed. 

Trichlorocyclotrithiazene, the cyclic trimer of thias l chloride, NSCl, is commonly prepared by the action of chlorine on S4N4 or S3N2C12 alternative preparation has been described involving the action of sulphuryl chloride on S4N4 or chlorocyclotrithiadiazonium chloride, S3N2C1+Q. The method is said to be more convenient and to yield a purer product. 

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. 

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. 

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... 

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-... 

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