Separating funnels

To extract the substance, the aqueous solution or suspension is placed in a separating-funnel, which may be either cylindrical. Fig. i6(a), or (better) pear-shaped, Fig. i6(b). Ether is then... 

For the separation of immiscible liquids a small separating funnel of the conventional type should be used whenever practicable, a pear-shaped funnel (Fig. 16, p. 35) of 5-10 ml. capacity being particularly... 

Ethyl bromide soon distils over, and collects as heavy oily drops under the water in the receiving flask, evaporation of the very volatile distillate being thus prevented. If the mixture in the flask A froths badly, moderate the heating of the sand-bath. When no more oily drops of ethyl bromide come over, pour the contents of the receiving flask into a separating-funnel, and carefully run oflF the heavy lower layer of ethyl bromide. Discard the upper aqueous layer, and return the ethyl bromide to the funnel. Add an equal volume of 10% sodium carbonate solution, cork the funnel securely and shake cautiously. Owing to the presence of hydrobromic and sulphurous acids in the crude ethyl bromide, a brisk evolution of carbon dioxide occurs therefore release the... 

When the solution has been boiling for hours, remove A, cool the contents, and then pour the ethanolic solution of the ester into a separating-funnel containing about 200 ml. of water, finally rinsing out the flask with a few ml. of water which are also doured into the funnel. Since the pensity of ethyl benzoate is only... 

Pour the mixture into a separating-funnel. Owing to the density of the acetate being only slightly greater than that of water, a sharp separation is usually not rapidly obtained. It is advisable therefore to add about 8 ml. of carbon tetrachloride, when, after shaking, a sharp and rapid separation of the heavy solution of the phenyl acetate in the... 

The crude acetonitrile contains as impurity chiefly acetic acid, arising from the action of phosphoric acid on the acetamide. Therefore add to the nitrile about half its volume of water, and then add powdered dry potassium carbonate until the well-shaken mixture is saturated. The potassium carbonate neutralises any acetic acid present, and at the same time salts out the otherwise water-soluble nitrile as a separate upper layer. Allow to stand for 20 minutes with further occasional shaking. Now decant the mixed liquids into a separating-funnel, run off the lower carbonate layer as completely as possible, and then pour off the acetonitrile into a 25 ml, distilling-flask into which about 3-4 g. of phosphorus pentoxide have been placed immediately before. Fit a thermometer and water-condenser to the flask and distil the acetonitrile slowly, collecting the fraction of b.p. 79-82°. Yield 9 5 g. (12 ml.). 

When the sodium has completely dissolved, pour the reaction-mixture into a separating-funnel, run off the strongly alkaline lower layer, and dry the upper layer over sodium sulphate not... 

Transfer the reaction-mixture to a separating-funnel, run off the aqueous layer, and collect the ethereal layer. Extract the aqueous layer twice with ether (2 x 25 ml.), add the extracts to the main ethereal solution and dry over sodium sulphate. 

This is done so that a small separating-funnel of about 100 ml. capacity may be used for the subsequent washing of the nitrobenzene. 

If only 100 ml. separating-funnels are available, the distillate must be divided into two portions and each extracted with ether as described, the final ether extracts being united for drying with potassium hydroxide. 

Dissolve 22-8 g. of ethyl crotonate in 40 ml. of dry carbon tetrachloride and add 35 6 g. of. V-bromosuccinimide. Heat the mixture under reflux for three hours. Cool to o and filter off the succinimide which is insoluble in cold carbon tetrachloride. Now shake the filtrate with water in a separating funnel, separate and dry the carbon tetrachloride layer with sodium sulphate. Filter through a fluted filter-paper into a Claisen flask and distil... 

Place the distillate in a separating-funnel and extract the benzonitrile twice, using about 30 ml. of ether for each extraction. Return the united ethereal extracts to the funnel and shake with 10% sodium hydroxide solution to eliminate traces of phenol formed by decomposition of the benzenediazonium chloride. Then run off the lower aqueous layer, and shake the ethereal solution with about an equal volume of dilute sulphuric acid to remove traces of foul-smelling phenyl isocyanide (CaHjNC) which are always present. Finally separate the sulphuric acid as completely as possible, and shake the ether with water to ensure absence of acid. Run off the water and dry the benzonitrile solution over granular calcium chloride for about 20 minutes. 

Now transfer the cold distillate to a separating-funnel, and shake vigorously with about 50-60 ml. of ether run oflF the lower aqueous layer and then decantf the ethereal solution through the mouth of the funnel into a 200 ml. conical flask. Replace the aqueous layer in the funnel, and extract similarly twice more with ether, combining the ethereal extracts in the conical flask. Add 3-4 g. of dry powdered potassium carbonate to the ethereal solution, securely cork the flask and shake the contents gently. The ethereal solution of the phenol... 

Suspend the crude hydrochloride in some water in a separating-funnel and add 20% sodium hydroxide solution until the mixture is definitely alkaline and the crude phenylhydrazine base floats as a deep red oil on the surface. Now extract the phenylhydrazine twice with benzene (using about 30 ml. of benzene on each occasion) and dry the united benzene extracts with powdered... 

Cool the reaction mixture, transfer it to a separating-funnel,... 

Chill the concentrated solution of the amine hydrochloride in ice-water, and then cautiously with stirring add an excess of 20% aqueous sodium hydroxide solution to liberate the amine. Pour the mixture into a separating-funnel, and rinse out the flask or basin with ether into the funnel. Extract the mixture twice with ether (2 X25 ml.). Dry the united ether extracts over flake or powdered sodium hydroxide, preferably overnight. Distil the dry filtered extract from an apparatus similar to that used for the oxime when the ether has been removed, distil the amine slowly under water-pump pressure, using a capillary tube having a soda-lime guard - tube to ensure that only dry air free from carbon dioxide passes through the liquid. Collect the amine, b.p. 59-61°/12 mm. at atmospheric pressure it has b.p. 163-164°. Yield, 18 g. 

Extract the dimethylaniline by shaking the distillate in a separating-funnel with a few ml. of ether, and then dry the ethereal solution over potassium carbonate distil the filtered ethereal solution from a small distilling-flask e.g, Fig. 36, p. 63) with the usual precautions, and finally the dimethylaniline, b.p. 193°. Yield, almost theoretical. 

Now cork the flask securely, and shake it vigorously for about 5 minutes the solution should now have only a faint brown colour due to unchanged iodine. Cool the mixture in ice-water, pour it into a separating-funnel, and extract it twice with water to remove sodium iodide and most of the ethanol. Then shake the residual ethereal solution with a dilute aqueoussolution of sodium thiosulphate the excess of iodine is thus removed and the... 

A 1500 ml. flask is fitted (preferably by means of a three-necked adaptor) with a rubber-sleeved or mercury-sealed stirrer (Fig. 20, p. 39), a reflux water-condenser, and a dropping-funnel cf. Fig. 23(c), p. 45, in which only a two-necked adaptor is shown or Fig. 23(G)). The dried zinc powder (20 g.) is placed in the flask, and a solution of 28 ml. of ethyl bromoacetate and 32 ml. of benzaldehyde in 40 ml. of dry benzene containing 5 ml. of dry ether is placed in the dropping-funnel. Approximately 10 ml. of this solution is run on to the zinc powder, and the mixture allowed to remain unstirred until (usually within a few minutes) a vigorous reaction occurs. (If no reaction occurs, warm the mixture on the water-bath until the reaction starts.) The stirrer is now started, and the rest of the solution allowed to run in drop-wise over a period of about 30 minutes so that the initial reaction is steadily maintained. The flask is then heated on a water-bath for 30 minutes with continuous stirring, and is then cooled in an ice-water bath. The well-stirred product is then hydrolysed by the addition of 120 ml. of 10% sulphuric acid. The mixture is transferred to a separating-funnel, the lower aqueous layer discarded, and the upper benzene layer then... 

During this period hydrogen chloride continues to be liberally evolved, and the product darkens considerably in colour. Now pour the product cautiously into 500 ml. of dilute hydrochloric acid and 100 g. of chipped ice in a separating-funnel, and shake the mixture thoroughly this operation removes the dark colour, and the toluene solution becomes yellow. Run off the lower acid layer, and extract the toluene three times with water. Finally dry the toluene solution over calcium chloride. 

Cool the mixture and pour the liquid reaction product into a separating-funnel. Rinse out the flask (which may contain some unchanged zinc) with ether, pour the latter into the funnel, and extract the aqueous solution with the ether. Repeat the extrac tion with a second quantity of ether, unite the ether extracts, wash them by extracting once with water, and then dry the ethereal extract over sodium sulphate. 

After 3 hours, replace the separating-funnel by a reflux condenser, and the thermometer by a stopper. Add 11 g. of zinc dust in small portions by rapid removal of the stopper at such a rate that the liquid is first brought to the boil (usually about 2 portions of 2 g. each) and is then maintained gently boiling. A ooid too rapid addition of the zinc, otherwise the reaction will become too vigorous, and rapid immersion of the flask in ice-water will be necessary to control the effervescence. 

Transfer the quinoline chlorozincate to a beaker, add a small quantity of water, and then add 10% sodium hydroxide solution until the initial precipitate of zinc hydroxide completely redissolves, and the free quinoline separates. Transfer the mixture to a separating-funnel, wash out the beaker with ether, adding the washings also to the solution in the funnel, and then extract the quinoline twice with ether. Dry the united ethereal extracts by adding an ample quantity of powdered potassium hydroxide and... 

Formation of nitrosaminey RgN NO. (a) From monomethylaniline. Dissolve I ml. of monomethylaniline in about 3 ml. of dil. HCl and add sodium nitrite solution gradually with shaking until the yellow oil separates out at the bottom of the solution. Transfer completely to a smdl separating-funnel, add about 20 ml. of ether and sh e. Run off the lower layer and wash the ethereal extract first with water, then with dil. NaOH solution, and finally with w ter to free it completely from nitrous acid. Evaporate the ether in a basin over a previously warmed water-bath, in a fume cupboard with no flames near. Apply Liebermann s reaction to the residual oil (p. 340). 

Place about 1 g. of the nitro-hydrocarbon in a boiling-tube and add 5 ml. of cone. HCl and several pieces of granulated tin. Warm the mixture and shake continuously to break up the oily drops of the nitro-compound. When all the oil has disappeared (about 3 minutes heating) pour off the liquid from any undissolved tin into a 100 ml. conical flask. Cool and add cautiously 30% aqueous NaOH solution until the precipitate formed redissolves to give a dark-coloured solution. Cool the latter thoroughly and shake well with about 15 ml. of ether. Separate the ethereal layer in a separating-funnel, wash with water and evaporate the ether in a basin on a previously heated water-bath in a fume-cupboard atoay from all flames. The residue is either... 

If no solid precipitate is obtained but the solution becomes cloudy, a low-melting or liquid phenol is indicated this will, of course, be revealed also by the characteristic phenolic odour. Transfer to a separating-funnel and extract with an equal volume of ether. Separate and dry with anhydrous sodium sulphate. Distil off the ether and identify the residue. 

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