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 Preparation of Phenyl(trichloromethyl)mercury
  • Preparation of Phenyl(trichloromethyl)mercury
  • Phenyl(trichloromethyl)mercury (CAS NO.: ) could be produced through the following synthetic routes.

    Preparation of Phenyl(trichloromethyl)mercury

    Into a 250-ml. round-bottomed flask equipped with a magnetic stirrer and reflux condenser fitted with a drying tube containing Drierite® are placed 150 ml. of dimethoxyethane, 27.8 g. (0.15 mole) of sodium trichloroacetate, and 31.3 g. (0.1 mole) of phenylmercuric chloride. The stirred mixture is heated to reflux (85°) by use of a heating mantle. dioxide evolution, which begins shortly after heating is begun. is accompanied by the appearance of a precipitate of sodium chloride. The reactants are heated at the reflux temperature until no more evolution is obvious (1 hour), then cooled to room temperature and poured into 500 ml. of water. The resulting mixture, consisting of a dense oil layer, a solid, and an aqueous layer, is extracted with four 50-ml. portions of diethyl ether. The combined ether layers are then washed with two 50-ml. portions of water, dried over anhydrous magnesium sulfate, filtered, and the solvent removed using a rotary evaporator. The resulting white solid, which weighs 44.8 g., is dissolved in 130 ml. of hot chloroform and fractionally crystallized. The first three fractions weigh 2.3 g. and are recovered phenylmercuric chloride. Successive reduction of solvent volume and further fractional crystallization provides 25.6 g. of product (65% yield), m.p. 110°.


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