Stannous sulfide, preparation

Stannic sulfide may be prepared as a yellow amorphous precipitate by double decomposition of a stannic salt with hydrogen sulfide. The crystalline modification, known as mosaic gold, may be prepared by sulfurizing stannous sulfide in the following way ... 

Chemical deoxygenation of sulfoxides to sulfides was carried out by refluxing in aqueous-alcoholic solutions with stannous chloride (yields 62-93%) [186 Procedure 36, p. 214), with titanium trichloride (yields 68-91%) [203], by treatment at room temperature with molybdenum trichloride (prepared by reduction of molybdenyl chloride M0OCI3 with zinc dust in tetrahydrofuran) (yields 78-91%) [216], by heating with vanadium dichloride in aqueous tetrahydrofuran at 100° (yields 74-88%) [216], and by refluxing in aqueous methanol with chromium dichloride (yield 24%) [190], A very impressive method is the conversion of dialkyl and diaryl sulfoxides to sulfides by treatment in acetone solutions for a few minutes with 2.4 equivalents of sodium iodide and 1.2-2.6 equivalents of trifluoroacetic anhydride (isolated yields 90-98%) [655]. 

Preparation. Thiophosgene forms from the reaction of carbon tetrachloride with hydrogen sulfide, sulfur, or various sulfides at elevated temperatures. Of more preparative value is the reduction of trichloromethanesulfenyl chloride [594-42-3] by various reducing agents, eg, tin and hydrochloric acid, stannous chloride, iron and acetic acid, phosphoms, copper, sulfur dioxide with iodine catalyst, or hydrogen sulfide over charcoal or silica gel catalyst (42,43). 

Amino-2,3-dihydro-l,4-phthalazinedione, also called luminol and 3-aminophthalhydrazide, has been prepared from 5-nitro-2,3-dihydro-1,4-phthalazinedione by reduction with ammonium sulfide or stannous chloride and by catalytic hydrogenation over palladium on charcoal in alkaline solution and by the reaction of 3-aminophthalimide with hydrazine hydrate. 

The detection of cations on chromatoplates is performed by spraying the solutions of the detection reagents at an appropriate concentration level, followed by visualization of the separated zones. The spraying reagents used as detectors include, 0.04-1 % dithizone in chloroform or carbon tetrachloride, 1% ethanolic solution of dimethylglyoxime, 1% aqueous solution of potassium ferrocyanide, 1% aqueous aluminon containing sufficient amount of ammonium acetate, 1% alcoholic solution of alizarine Red S, freshly prepared 0.1% solution of stannous chloride in 2 M HCl, hydrogen sulfide gas, aqueous saturated solution of ammonium sulfide, aqueous solution of ammonium thiocyanate and dilute solutions of diphenylcarbazide, p-nitroso-yV,A -dimethylaniline and sodium rhodizonate. 

Preparation of derivatives for chromatography To a solution of 0.5 mmole of sulfide in 2 ml of methanol a solution of 200 mg of sodium p-nitrobenzenesulfochloroamide in 5 ml of methanol is added and the reaction mixture is suitably acidified with one drop of 1% formic acid in methanol (to make the reaction smoother). The reaction is accompanied by decolorization of the yellow reaction mixture. After 15 min the reaction mixture is diluted with 20 ml of water and additioned with 10 ml of 2 N NaOH. It is then extracted twice with 5 ml of chloroform. The chloroform solution is applied directly onto the paper, a suitable amount being 5 to 15 ig. Detection is carried out by spraying the chromatogram with a solution of p-dimethylaminobenzaldehyde after previous reduction with stannous chloride (p. 154). Yellow spots on a white background are produced. 

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