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Diethyl from tellurium, sodium/liquid ammonia

Divinyl Ditellurium2 To 4.1 g (22.6mmol) divinyl tellurium in 200m/ liquid ammonia is added 1.02 g (44.3 mmol) of sodium in small pieces. The ammonia is evaporated after 40 min, 150 m/water is added to the residue, and the mixture is extracted with three 50-m/ portions of diethyl ether. The combined extracts are washed with water and dried with anhydrous magnesium sulfate. The mixture is filtered, and the diethyl ether removed from the filtrate at reduced pressure. Divinyl dilellurium remained as a red-brown oil yield 70%. [Pg.265]

Dibenzylidene-l,3-ditelluretane1- 3 Under an inert atmosphere, 1.15 g (50 mmol) of sodium are dissolved in 250 ml of liquid ammonia (freshly distilled from sodium). A small amount of iron(III) nitrate is added to the ammonia solution and then 5.1 g (50 mmol) of phenylacetylene are added dropwise to the stirred sodium amide solution over 30 min. The mixture is allowed to stand for 30 min, 6.4 g (50 mmol) of finely powdered tellurium are added, and the ammonia is evaporated from the mixture under protection against atmospheric moisture. Residual liquids are evaporated under vacuum. The residue (sodium phenylethyneteUuiolate) is dissolved in 50 ml of absolute dimethyl sulfoxide and the solution is cooled to 0°. Under continuous cooling, 25 ml of a 2 molar solution of hydrogen chloride in diethyl ether is added slowly. The precipitate is filtered off, washed with water, chloroform, and then recrystallized from dimethylformamide to give the trans-isomer yield 4.3 g (38%) m.p. 270-275°. [Pg.727]


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