Separation of water-insoluble mixtures

TABLE XI,9,1. GENERAL SCHEME FOR SEPARATION OF A WATER-INSOLUBLE MIXTURE... 

About 5 minutes later, the liquid contents of the beaker are poured cautiously into a 2-1. glass beaker, and this is tipped and rotated slowly so as to spread the congealing mass in a thin film on the beaker walls. When the material in the beakers has cooled, a total of 11. of water is poured into the beakers and the water is stirred well for at least 1 hour (Note 5). The cold suspension is filtered with suction to separate 200-210 g. of an insoluble mixture of lead monoxide and red lead, which is washed on the filter with six 50-ml. portions of water. 

C. p-Bromodiphenylmethane. A 2-1. three-necked flask fitted with a distillation condenser, a thermometer, and an efficient mechanical stirrer is charged with 1.1 1. of diethylene glycol (Note 7) and a solution of 190 g. of potassium hydroxide in 100 ml. of water. The mixture is stirred, and water is distilled until the internal temperature reaches 180°. The resulting solution is allowed to cool to 100° or below, and 146 g. (0.40 mole) of l-/>-bromophenyl-l-phenyl-2,2,2-trichloroethane (Note 8) is added. The condenser is set for reflux, and the mixture is stirred and heated to boiling for 5 hours (Note 9). The hot solution is then poured onto 3 kg. of cracked ice, and the mixture is allowed to stand overnight. The oily layer is separated and dissolved in ether (any insoluble material is discarded), and the aqueous layer is extracted with 250 ml. of ether. The combined ethereal solution and extracts are dried over calcium chloride and filtered. The ether is removed under reduced pressure on a hot water bath. The product is distilled under reduced pressure b.p. 120-130° (3 mm.), 155-163° (13 mm.) (Note 10), n2id 1.6028, dH 1.342. The yield is 74-79 g. (75-80%) (Note 11). 

Table 9.3 General scheme for separation of a water-insoluble mixture...

General scheme for separating a simple mixture of water-insoluble compounds. 

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