Potassium sulfide, preparation solution

A solution is prepared by diluting 0.7850 L of 1.262 M potassium sulfide solution with water to a final volume of2.000 L. 

Prepare 50 cc. of a 5 per cent solution of potassium hydroxide. Divide this into two equal parts saturate the one with hydrogen sulfide and add it to the other. This gives a solution of potassium sulfide. Place the solution in a small flask, add 2 cc. of carbon disulfide, and shake thoroughly for some time. After about 5 min., filter through a wet filter. The orange-red solution contains K2CS3 and is a very sensitive reagent toward nickel. Make tests especially in the presence of cobalt. 

Thiobenzophenone has been prepared by the action of thio-phosgene on benzene in the presence of aluminum chloride 1 by the action of phosphorus pentasulfide on benzophenone 2 by the action of alcoholic potassium sulfide on benzophenone dichloride 3 by treating benzophenone dichloride with an alcoholic solution of sodium hydrosulfide 4 and by the action of thioacetic acid on benzophenone dichloride.5... 

Both anhydrous and hydrated sodium or potassium sulfide in ethanol have been used in the synthesis of thietanes. A common procedure is to use a solution of sodium or potassium hydroxide saturated with hydrogen sulfide. Liquid ammonia has been used as a solvent for the preparation of thietane (32%) from sodium sulfide and 1,3-dibromopropane. Phase-transfer catalysis has been used to good effect.A variation in which l,3-dichloro-3-methylbutane 3 is treated with aluminium chloride and hydrogen sulfide followed by aqueous sodium hydroxide gave 2,2-dimethylthietane 4 in 90% yield. An intermediate aluminium chloride-alkene complex, 5 or 6, was proposed. 

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. 

The common method for preparing CuNs is by reaction of a cuprous salt with sodium azide. Aqueous solution of cupric salt (sulfate) is reduced with potassium sulfide giving cuprous sulfide as precipitate which is then dissolved by addition of acetic acid. In the following step, sodium azide is added to the solution, precipitating CuNs [78,107]. 

A solution of 64.9 g. (I mole) of 86.5% potassium hydroxide (Note I) in 28 ml. of water is cooled in an ice bath, saturated with hydrogen sulfide, and flushed with nitrogen to ensure complete removal of excess hydrogen sulfide (Notes 2 and 3). The freshly prepared potassium hydrosulfide solution is diluted with 117 ml. of water and stirred under nitrogen at 55-60°. Then 95.3 g. (0.5 mole) of finely ground tosyl chloride (Note 3) is introduced in small portions at a uniform rate so that the reaction temperature is maintained at 55-60° (Note 2). A mildly exothermic reaction ensues, and the solution becomes intensely yellow. After about 90 g. of tosyl chloride has been introduced, the yellow color disappears, and the dissolution of the chloride ceases. The reaction mixture is rapidly filtered with suction through a warmed funnel, and the filtrate is cooled several hours at 0-5°. The crystals of potassium... 

Interaction of substituted arenediazonium salts with potassium O. O-diphenylphosphorodithioates gave a series of solid diazonium salts which decomposed explosively when heated dry [10], The unique failure of diazotised anthranilic acid solutions to produce any explosive sulfide derivatives under a variety of conditions has been investigated and discussed [6]. Preparation of diaryl sulfides from interaction of diazonium and thiophenoxide salts led to violent explosions, attributed to presence of some arenediazo sulfide during subsequent distillation of the diaryl sulfides. Precautions are detailed [11]. A safe method of preparation of diaryl sulfides from diazonium tetralluoroborates and sodium benzenethiolate in DMF is now available [12],... 

Red sulfide occurs natively and is mined from mineral cinnabar. Also it can be prepared by beating mercury with a solution of potassium pentasulfide, producing a scarlet cinnabar ... 

Potassium chlorate is an oxidizing agent in matches, fireworks and explosives. The head of safety matches is coated with potassium chlorate which is struck on a surface consisting of red phosphorus, antimony(lII) sulfide and an adhesive to light the fire. It also is used in laboratory preparation of oxygen. Its dilute aqueous solution is an antiseptic. 

Three and four-tenths grams of antimony trisulfide is prepared by passing hydrogen sulfide into a solution of 6.6g potassium antimonyl tartrate (4.5g of the trichloride or 2.9g of the trioxide may be used instead) in 2N hydrochloric acid until precipitation is complete. 

The synthesis of 2C-T-17 R required starting with the S isomer of secondary butanol. The S 2-butanol in petroleum ether gave the lithium salt with butyllithium which was treated with tosyl chloride (freshly crystallized from naphtha, hexane washed, used in toluene solution) and the solvent was removed. The addition of 2,5-dimethoxythiophenol, anhydrous potassium carbonate, and DMF produced S 2,5-dimethoxyphenyl s-butyl sulfide. The conversion to R 2,5-dimethoxy-4-(s-butyl-thio)benzaldehyde (which melted at 78-79 °C compared to 86-87 °C for the racemic counterpart) and its conversion in turn to the nitro-styrene, S -2,5-dimethoxy-4-(s)-butylthio-B-nitrostyrene which melted at 70-71 °C compared to 68-69 °C for the racemic counterpart, followed the specific recipes above. The preparation of the intermediates to 2C-T-17 S follows the above precisely, but starting with R 2-butanol instead. And it is at these nitrostyrene stages that this project stands at the moment. 

During preparation of thiophenol by addition of a cold solution of potassium O-methyldithiocarbonate to a cold solution of benzenediazonium chloride, a violent explosion accompanied by an orange flash occurred [1], This was attributed to the formation and decomposition of bis(benzenediazo) disulfide. A preparation in which the diazonium solution was added to the xanthate solution proceeded smoothly [2], See also DIAZONIUM SULFIDES AND DERIVATIVES... 

Mercaptopyrazine (151a) is best prepared by the action of sodium hydrogen sulfide on chloropyrazine in dimethylformamide.147 It decomposes on heating with evolution of hydrogen sulfide and formation of di-2-pyrazinyl sulfide. The latter compound is also obtained together with mercaptopyrazine on treatment of chloropyrazine with aqueous potassium hydrogen sulfide solution. Comparison of the... 

Preparation. The sulfurane (I) is prepared most conveniently in nearly quantitative yield by treatment of an ethereal solution of the [>ota sium salt of hexafluoro-2-phenyl-2-propanol (RfOH, prepared by the reaction of the alcohol with potassium metal) and diphenyl sulfide with chlorine at - 78°. Removal of the potassium chloride by filtration and of the ether by evaporation under vacuum leaves the white, crystalline sulfurane (I), which can be crystallized from pentane. Moisture must be avoided... 

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