2- phenyl tellurium chloride

Phenylazo)phenyl tellurium chloride reacted with sodium dithiocarbamates at room temperature to give 2-(phenylazo)phenyl dithiocarbamato tellurium compounds3. 

Phenylazo)phenyl Dialkyldithiocarbamato Tellurium3 A solution of the sodium dialkyldithiocarbamate (1.03 mmol) in 15 ml dry methanol is added under an atmosphere of nitrogen to a stirred solution of 2-(phenylazo)phenyl tellurium chloride (0.35 g, 1.0 mmol) in dichloromethane (25 ml). The mixture is stirred for 20 min at 20°. The solvents are removed on a rotary film evaporator. Dichloromethane is added to the residue. The mixture is vigorously stirred and the solution is filtered to remove the sodium chloride. 

A similar exchange reaction produced the 1 1 complexes of phenyl tellurium thiocyanate with ethylenethiourea1, when the phenyl tellurium chloride complex was treated with potassium thiocyanate in aqueous methanol. However, the phenyl tellurium chloride -selenourea adduct and potassium selenocyanate yielded bis[phenyIteUuro] selenium3. Phosphane selenides also coordinate to phenyl tellurium halides3. 

Phenylazo)phenyl tellurium chloride and sodium acetate produced the expected aryl tellurium acetate4 (p. 238). 

Phenylazo)phenyl tellurium chloride and ammonium thiocyanate yielded the aryl tellurium thiocyanate5 (p. 204). 

Phenyl thiourea tellurium nitrate and perchlorate were isolated when nitric or perchloric acid were added to aqeuous solutions containing phenyl tellurium chloride and thiourea. 

Phenylazo)phenyl tellurium chloride and ammonium thiocyanate yielded 2-(phenylazo)phenyl tellurium thiocyanate. This compound is stabilized through coordination of the azo group to tellurium3 (see p. 202 ff). 

Phenylazo)phenyl Tellurium Thiocyanate Under an atmosphere of nitrogen, a solution of 152 mg (2 mmol) of ammonium thiocyanate in 40 ml dry methanol is slowly added to a stirred, refluxing mixture of 688 mg (2 mmol) of 2-(phenylazo)phenyl tellurium chloride and 50 ml dichloromethane. With constant stirring, the mixture is refluxed for 5 min after completion of the addition and then cooled to 20°. The solvents arc removed on a rotary evaporator. 200 ml dichloromethane are added, the mixture is vigorously stirred, and then filtered to remove insoluble ammonium chloride. The solvent is removed from the filtrate on a rotary evaporator. The residue is stirred with 8 ml methanol and then filtered. The filter cake is recrystallized from methanol to give orange-red crystals yield 60% m.p. 122° (dec.). 

Methoxy phenyl Tellurium Chloride Benzenesulfonimide b To 3 0 m/ of carbon tetrachloride are added 1.17 g (2.5 mmol) of bis[4-methoxyphenyl] ditellurium, the solution is cooled to - 10 with stirring, and 0.19 g (2.7 mmol) of chlorine dissolved in 5 ml of carbon tetrachloride are added. The mixture is stirred for 20 min, warmed to 20°, and a solution of 0.29 g (1.3 mmol) of A,A-diehlorobenzenesulfonamide in 40 ml of carbon tetrachloride is added. The mixture is allowed to stand overnight and is then filtered. The solid is washed with several 5 w/portions of diethyl ether/dioxane (5/1, v/v) and the remaining solid is recrystallized from dioxane or toluene yield 0.41 g (78%) m.p. 202°. 

Phenylazo)phenyl tellurium acetate was prepared from the aryl tellurium chloride and sodium acetate. The tellurium atom is in a trigonal bipyramidal environment with the oxygen and one nitrogen atom in the two axial positions1. 

The possibility of preparing aryl tellurium halides from equimolar amounts of diaryl ditellurium compounds and aryl tellurium trihalides has hardly been explored. Only phenyl tellurium iodide and 2-biphenylyl tellurium bromide could be obtained by this route. The other aryl tellurium halides (including 3,4-dimethoxyphenyl tellurium chloride) decomposed under the reaction conditions to give diaryl tellurium dihalides and tellurium5. 

When the thiosemicarbazones of benzaldehyde, 2-hydroxybenzaldehyde, methyl phenyl ketone, or methyl 2-hydroxyphenyl ketone were reacted with aryl tellurium trichlorides, reduction to the aryl tellurium chlorides occurred. The aryl tellurium chlorides were stabilized by coordination to excess thiosemicarbazone2. 

Benzoylphenyl Tellurium Chloride1 In a dry, 100 m/ flask fitted with a reflux condenser topped with a drying tube are placed 6.5 g (20 mmol) of 2-carboxyphenyl phenyl tellurium, 5 ml (30 mmol) of butyl dichloromethyl ether, and 0.2 g (1.5 mmol) of anhydrous zinc chloride. The mixture is heated on a boiling water bath for 2 h, then diluted with carbon tetrachloride, charcoal is added, and the mixutre is filtered. The filtrate is evaporated to dryness and the residue is recrystallized from benzene/hexane yield 6.3 g (80%) m.p. 113-114°. 

However, 2-methyl-3-phenyl (or 2,3-diphenyl)-3-oxo-prop-l-en-1-yl tellurium chloride did not react with aqueous ammonia nor with triethylamine10. 

Sulfuryl chloride and diphenyl ditelluriumin chloroform gave phenyl tellurium trichloride in 80% yield3. 

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). 

Methoxyphenyl Tellurium Trilluoride1 A 100 ml two-necked flask fitted with a magnetic stirrer and a reflux condenser is charged with 1.3 g (6 mmol) of silver fluoride and 30 ml of dry toluene. The stirred suspension is heated to reflux, 0.68 g (2 mmol) of 4-methoxyphenyl tellurium trichloride are added in small portions, and refluxing is continued for 3 h. The mixture is allowed to cool to 20°, silver chloride is filtered off, and fight petroleum is added to the filtrate. The precipitated product is collected and dried m.p. 176 178 . 4-Ethoxy phenyl tellurium trifluoride (m.p. 204°) was similarly prepared. 

Phenyl tellurium trichloride and triarylarsane dioximates reacted with replacement of one chloride for a dioximate group1. 

When phenyl tellurium trichloride or 4-phenoxyphenyl tellurium trichloride were reacted with sodium 2-benzoyl-5-methoxyphenoxide in a refluxing mixture of benzene/methanol, compounds were obtained that contained chloride and phenoxide groups3. 

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