Sodium sulfide, nonahydrate

An exotherm is witnessed and the temperature rises to 70-80°. A color change from yellow to deep purple is also seen the extent of coloration varies with the purity of the sodium sulfide nonahydrate. 

The amount of sodium sulfide nonahydrate needed varies from 12 to 25 g. from one run to another. 

Sodium phenoxide, 32, 75 33, 43, 45 Sodium sulfhydrate, 31, 7 Sodium sulfide nonahydrate, 31, 6 Sommelet reaction, 33, 93 Sorbic acid, S-hydroxy-0-methyl, 3-lactone, 32, 57 Stannic chloride, 33, 91 Stearone, 33, 84 ms-Stilbene, 33, 88 Irans-Stilbene, 33, 89... 

TAT, Nitric acid. Phosphorus pentoxide Resorcinol, Nitric acid. Sodium nitrite. Sulfuric acid Resorcinol, Nitric acid. Sodium nitrite Diethyl ether, Dichloromethylphosphine, Ethyl alcohol, N,N-Diethylamine, 2-Ethylthioethanol, Rhombic sulfur Ethylene Chlorohydrin, Sodium sulfide, Nonahydrate, Hydrochloric acid... 

Sodium metapenodate, 55, 68 Sodium methanesulfinate, 57, 88 Sodium-potassium alloy, 57, 5 Sodium sulfide, nonahydrate, 57, 55... 

Sodium sulfide nonahydrate reduced 2-acyloxy-3-chloropropyl tellurium trichlorides1 and 2-chloroethenyl tellurium trichloride2 to the ditellurium compounds without affecting the other functional groups in the molecules. 

Bis[2-benzoyloxy-3-chloropropyl] Ditellurium1 In a 250 ml separatory funnel are placed 0.80 g (1.85 mmol) of 2-benzoyloxy-3-chloropropyl tellurium trichloride, 40 ml of dichloromethane, and 30 ml of 20% (w/v) aqueous sodium sulfide nonahydrate solution. The mixture is shaken until all solids have dissolved, the organic layer is separated, dried, and the solvent evaporated. The product is purified by passing it through a short column of silica with dichloromethane as the mobile phase. The orange-red colored fractions are evaporated to leave a red oil yield 0.48 g (80%). 

Bis[4-propoxyphenyl] Ditellurium [Sodium Sulfide Method]5 3.7 g (0.01 mol) of 4-propoxyphenyl tellurium trichloride are thoroughly ground with 20 g (0.08 mol) of sodium sulfide nonahydrate, the mixture is heated with stirring on a boiling water bath for 30 min, cooled to 20°, and mixed with ice/watcr. The product is extracted with petroleum ether, the extract is evaporated, and the residue is recrystallized from petroleum ether yield 2.3 g (86%) m.p. 84°. 

Phenyl Tellurium Trichloride1 A mixture of 0.9 g (2.6 mmol) of diphenyl tellurium dichloride, 1.38 g (5.1 mmol) of tellurium tetrachloride, and 10 m/ of toluene is heated under reflux for 12 h. The solvent is removed under vacuum, 14.4 g (60 mmol) of sodium sulfide nonahydrate are added to the residue, the mixture is heated at 95-100° on a boiling water bath for 25 min, and cooled. Water is added and the mixture is extracted with chloroform. The chloroform extract is dried with anhydrous calcium chloride, most of the chloroform is distilled, and a solution of 1.0 g (8.4 mmol) of thionyl chloride in chloroform is added dropwise to the vigorously stirred, concentrated solution of diphenyl di tellurium while the flask is cooled in an ice bath. Petroleum ether is added to the resulting mixture to precipitate the product yield of crude product 1.1 g (69%) m.p. 211-214° (1,1,2,2-tetrachloroethane). 

Chloroethyl tellurium trichlorides heated with sodium sulfide nonahydrate to 100° formed ethenes2,4. The detelluration step is a slereospecific /rani-elimination, which, together with the syn-addition of tellurium tetrachloride to the olefin, results in an inversion of the olefin4. 

Reaction of Diorgano Tellurium Dihalides with Sodium Sulfide General Procedure A 15-fold molar excess of sodium sulfide nonahydrate is mixed with the diorgano tellurium di halide and the mixture is heated at 90-95° on a boiling water bath. When the mixture has become liquid, it is stirred for an additional 10 min. and then cooled. Water is added to dissolve the sulfide and the mixture is filtered to collect the solid diorgano tellurium product. Liquid diorgano tellurium products are extracted into petroleum ether. Products are purified by recrystallization or distillation. 

Heating powdered tellurium with 1,2-diiodotetrafluorobenzene in an evacuated tube at 300° produced octafluorotelluranthrene in 30% yield. In order to purify the telluranthrene, it was converted to the tetrabromide. Reduction of the tetrabromide with sodium sulfide nonahydrate gave the pure telluranthrene. 

Merck s reagent grade of sodium sulfide nonahydrate was used. Since sodium sulfide decomposes on contact with air, a freshly opened bottle should be employed. Sodium Sulfhy-drate (Hooker Electrochemical Company hydrated sodium hydrosulfide) is also satisfactory the amount should be based upon the formula NaHS 2H20, and an equivalent amount of sodium hydroxide in excess of the 27 g. is required. 

A mixture of 128 g. (0.81 mole) of p-chloronitrobenzene and a solution of 480 g. (2.0 moles) of sodium sulfide nonahydrate in 2 1. of water is heated to reflux for 8 hours. The cooled mixture is extracted with ether to remove a small amount of oil, the remaining aqueous solution is saturated with sodium chloride, and 240 g. (4.0 moles) of glacial acetic acid is added. The precipitated oil is removed by... 

A mixture of 1.5 1. of water, 240 g. (1.0 mole) of sodium sulfide nonahydrate, and 64 g. (2.0 gram atoms) of sulfur is stirred until the sulfur dissolves. After filtration the solution is added (10-15 minutes) with stirring to a solution of 242 g. (1.02 moles) of cobalt chloride hexahydrate in 1.7 1. of water. Stirring is continued for an additional... 

Fifty milliliters of 95% ethanol is heated to reflux in a flask equipped with two dropping funnels, a stirrer, and a condenser. In one funnel is placed 54 g. (0.25 mole) of tetramethylene bromide (p. 271) in 100 ml. of ethanol, and in the other a solution of 60 g. (0.25 mole) of sodium sulfide nonahydrate in a mixture of 100 ml. of ethanol and 50 ml. of water. The two solutions are added at such a rate that the additions are completed at the same time. About 3 hours is required to add the reagents, and the mixture is stirred and heated under reflux for an additional 6 hours. The same amounts of reagents... 

The reduction of alkyl tellurium tri halides is a convenient method for the preparation of the corresponding dialkyl ditellurium when the trihalides can be obtained by reactions other than the halogenolysis of the dialkyl ditellurium. Addition of tellurium tetrachloride to olefins and condensation with ketones produces alkyl tellurium trichlorides. Sodium sulfide nonahydrate" and sodium or potassium disulfite were used as reducing agents. 

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