Bolt-head flasks

The crude material is therefore placed either in a round-bottomed bolt-head flask (Fig. 8) or in a conical flask, the solvent added (again in slight deficiency) and a reflux water-condenser fitted to the flask as shown. The mixture is boiled either on a water-bath or over a gauze, and then more solvent added cautiously down the condenser until a clear solution (apart from insoluble impurities) is again obtained. It is then filtered hot as described above. 

The crude organic material is placed in a porous thimble G (made of tough filter-paper), and the latter placed as shown within the inner tube C. The apparatus is then fitted below to a bolt-head flask H containing the requisite solvent, and above to a reflux water-condenser J. 

Fit a 500 ml. bolt-head flask F with a well-fitting cork which is free from flaws, and which carries a dropping-funnel D and a delivery tube (or knee-tube ) T, the latter being connected to a water-condenser C (Fig. 52). Attach an adaptor A to the lower end of the condenser. (Alternatively, use a ground-glass flask (Fig. 22(a), p. 43) with a distillation-head (Fig. 22(F)) the dropping-funnel can be fitted into the distillation-head, the side-arm of which is connected to a condenser as in Fig. 23(0), p. 45.)... 

Fit a 50 ml. bolt-head flask F (Fig. 53) with a reflux water-condenser C, to the top of which a dropping-funnel D is fixed by means of a cork having a vertical V-shaped groove G cut or filed in the side to... 

To prepare pure acetylene, assemble the apparatus shown in Fig. 57. F is a wide-necked 300 ml. bolt-head flask, to which is fitted a double-surface reflux water-condenser C and the dropping-funnel D. From the top of C, a delivery-tube leads down to the pneumatic trough T, where the gas can be collected in jars in the usual way. (Alternatively, use the apparatus shown in Fig. 23(A),... 

Assemble the apparatus shown in Fig. 6o. A is a 500 ml. bolt-head flask connected by a knee-tube B to a water-condenser C, to the lower end of which is fitted the adaptor D. In view of the low boiling-point of the ethyl bromide, it is essential that the various portions of the apparatus are connected together by well-bored, tightly fitting corks. (For this reason, the apparatus shown in Fig. 23(0), p. 45, is preferable.)... 

When all the sodium nitrite has been added and diazotisation is complete, transfer the cold solution to a 600 ml. round-bottomed bolt-head flask. Dissolve 35 g. of potassium iodide in 50 ml. of water, and add this solution slowly with shaking to the cold... 

Add 23 g. of powdered (or flake ) sodium hydroxide to a solution of 15 ml. (18 g.) of nitrobenzene in 120 ml. of methanol contained in a 250 ml. short-necked bolt-head flask. Fix a reflux water-condenser to the flask and boil the solution on a water-bath for 3 hours, shaking the product vigorously at intervals to ensure thorough mixing. Then fit a bent delivery-tube to the flask, and reverse the condenser for distillation, as in Fig. 59, p. 100, or Fig. 23(D), p. 45). Place the flask in the boiling water-bath (since methanol will not readily distil when heated on a water-bath) and distil off as much methanol as possible. Then pour the residual product with stirring into about 250 ml. of cold water wash out the flask with water, and then acidify the mixture with hydrochloric acid. The crude azoxybenzene separates as a heavy oil, which when thoroughly stirred soon solidifies, particularly if the mixture is cooled in ice-water. 

Dissolve 1 g. of anthracene in 10 ml. of glacial acetic acid and place in 50 ml. bolt head flask fitted with a reflux water-condenser. Dissolve 2 g. of chromium trioxide in 2 ml. of water and add 5 ml. of glacial acetic acid. Pour this solution down the condenser, shake the contents of the flask and boil gently for 10 minutes. Cool and pour the contents of the flask into about 20 ml. of cold water. Filter off the crude anthraquinone at the pump, wash with water, drain well and dry. Yield, 1 g. Purify by re crystallisation from glacial acetic acid or by sublimation using the semi-micro sublimation apparatus (Fig. 35, p. 62, or Fig. 50, p. 70). 

Fit a 750 ml, bolt-head flask (also by a rubber stopper) to a reflux water-condenser closed at the top by a calcium chloride tube ensure that flask and condenser are quite dr). Place 150 ml. of the dried ethyl acetate in the flask and add 15 g. of sodium. The sodium for this purpose should preferably be added in the form of wire directly from a sodium press (Fig. 55, p. 82) alternatively the sodium may be added as thin slices, but in this case each slice should be quickly pressed between drying-paper before being added to the acetate to remove the wet film which may have formed during the weighing and cutting of the metal. 

Oxidation, (i) Dissolve 5 g. of potassium dichromate in 20 ml. of dil. H2SO4 in a 100 ml. bolt-head flask. Cool and add 1 ml. of methanol. Fit the flask with a reflux water-condenser and warm gently a vigorous reaction soon occurs and the solution turns green. The characteristic pungent odour of formaldehyde is usually detected at this stage. Continue to heat for 3 minutes and then fit the flask with a knee-tube (Fig. 59, p. 100) and distil off a few ml. Test the distillate with blue litmus-paper to show that it is definitely acid. Then apply Test 3 p. 350) for formic acid. (The reflux-distillation apparatus (Fig. 38, p. 63) can conveniently be used for this test.)... 

A common operation in practical organic chemistry is for stirring, refluxing, and addition of a liquid from a dropping funnel to be carri on simultaneously. The most convenient apparatus for this purpose is a three-necked flask, fitted as in Fig. 11, 7, 11, a. If a three-necked flask is not available, the three-way adapter inserted into a bolt-head flask (Fig. 77, 7, 11, 6) may be used. A further simplification, suitable for elementary students, is to employ a two-way adapter as in Fig. 77, 7, 11, c the stirrer passes through a closely-fitting glass sleeve which is extended... 

Fig. II, 16, 1 illustrates a set-up for simple fractionation a Hempel column is shown, but it may be substituted by a modified Hempel, a Vigreux or an all-glass Dufiton column. The Hempel column may be filled with glass rings, h porcelain Lessing rings, or with porcelain rings. The mixture to be fractionated is placed in a bolt - head flask of convenient size (it should be one third to one half full), a few fragments of porous porcelain added, the column fixed in position, and a water condenserattacfied to the side arm. The distillate is collected in small flasks or in test tubes. The bulb of the thermometer should be just below the level of the side arm.

The steam distillation of small quantities of material may be conducted in the apparatus of Fig. 11, 41, 5. The substance to be distilled is placed in the small inner tube (a specially constructed test-tube) and water is boiled in the outer bolt-head flask. The volume of the liquid in the inner tube does not increase appreciably since it is immersed in the hot liquid in the flask. 

Flasks. Round-bottomed, flat-bottomed, conical (Erlenmeyer) and bolt-head flasks up to a capacity of 2-3 litres are generally fitted with a 524 socket f those from 5 to 100 ml. are available with a 514 or 519 (from 25 ml.) socket. Round- and flat-bottomed flasks exceeding 1 litre in capacity are supplied with 534 necks. Whilst all sizes of sockets can be obtained from the manufacturers, it is usually convenient to limit the socket sizes to a small number (say, 514, 519, 524 and 534), thus per mitting interchangeability with the minimum number of adapters. 

Sulphuric acid method. Place 20 g. of commercial cycZohexanol and 0-6 ml. of concentrated sulphuric acid in a 150 or 200 ml. round-bottomed or bolt head flask, add 2-3 chips of porous porcelain, and mix well. Fit the flask with a fractionating column, a Liebig condenser, adapter and filter flask receiver as in Section 111,10 (1). Heat the flask in an air bath (Fig. II, 5, 3) at such a rate that the temperature at the top of the column does not rise above 90° alternatively, an oil bath, heated to a temperature of 130-140°, may be used. Stop the distillation when only a small residue remains and the odour of sulphur dioxide is apparent. Transfer the distillate to a small separatory funnel. 

The small capacity apparatus is especially recommended for the use of students the consumption of iodine by a large class of students is not unreasonably high. Larger apparatus, e.g., 60 ml. and 100 ml. capacity holding 100 g. and 200 g. respectively of iodine, are generally preferred for routine preparations of alkyl iodides the bolt-head flask should then be of 250 or 500 ml. capacity. Thus for n-butyl iodide a typical preparation would employ 120 g. (148-5 ml.) of n.butyl alcohol, 21 75 g. of red phosphorus, and 200 g. of iodine. 

The yields, unless otherwise stated, exceed 90 per cent, of the theoretical. The appropriate size of apparatus (generally of 60 ml. or 100 ml. capacity) should be used ths corresponding bolt.head flask should have a capacity of 250 or 500 ml. 

Fit up the apparatus shown in Fig. Ill, 61, 1. The bolt-head flask is of 500 ml. capacity and the Hempel column is fllled with glass rings... 

Place a mixture of 53 g. of A.R. lactic acid (85-88 per cent, acid), 75 g. (85-5 ml.) of commercial anhydrous isopropyl alcohol, 300 ml. of benzene and 20 g. of Zeo-Karb 225/H (1) in a 700 ml. bolt-head flask, equipped with an automatic water separator (e.g., a large modified Dean and Stark apparatus with a stopcock at the lower end, see Fig. Ill, 126, 1) carrying an efficient reflux condenser at its upper end, and a mercury-sealed stirrer (alternatively, the hquid-sealed stirrer shown in Fig. 11,7,11, c. may be used). Reflux the mixture, with stirring, on a steam bath for 5 hours or until water no longer collects in appreciable amount in the water separator run off the water from time to time. Filter off the resin at the pump and wash it with two 25 ml. portions of benzene. Shake the combined filtrate and washings with about 5 g. of precipit-ated calcium... 

Furfuryl acetate. Reflux a mixture of 39 2 g. (34-8 ml.) of redistilled furfuryl alcohol, 48 g. of glacial acetic acid, 150 ml. of benzene and 20 g. of Zeo-Karb 225/H in a 500 ml. bolt-head flask, using the apparatus described under iaoPropyl Lactate. After 3 hours, when the rate of collection of water in the water separator is extremely slow, allow to cool, separate the resin by suction filtration, and wash it with three 15 ml. portions of benzene. Remove the benzene, etc., from the combined filtrate and washings under reduced pressure (water pump) and then collect the crude ester at 74-90°/10 mm. a small sohd residue remains in the flask. Redistil the crude ester from a Claisen flask with fractionating side arm pure furfuryl acetate passes over at 79-80°/17 mm. The yield is 14 -5 g. 

Fit a 1500 ml. bolt-head flask with a reflux condenser and a thermometer. Place a solution of 125 g. of chloral hydrate in 225 ml. of warm water (50-60°) in the flask, add successively 77 g. of precipitated calcium carbonate, 1 ml. of amyl alcohol (to decrease the amount of frothing), and a solution of 5 g. of commercial sodium cyanide in 12 ml. of water. An exothermic reaction occurs. Heat the warm reaction mixture with a small flame so that it reaches 75° in about 10 minutes and then remove the flame. The temperature will continue to rise to 80-85° during 5-10 minutes and then falls at this point heat the mixture to boiling and reflux for 20 minutes. Cool the mixture in ice to 0-5°, acidify with 107-5 ml. of concentrated hydrochloric acid. Extract the acid with five 50 ml. portions of ether. Dry the combined ethereal extracts with 10 g. of anhydrous sodium or magnesium sulphate, remove the ether on a water bath, and distil the residue under reduced pressure using a Claiseii flask with fractionating side arm. Collect the dichloroacetic acid at 105-107°/26 mm. The yield is 85 g. 

Tribromoaniline. Assemble the apparatus depicted in Fig. 7F, 47, 1. The distilling flask B has a capacity of 100 ml. and the bolt-head flask A (which may be replaced by a flat-bottomed flask) is 1 litre. Into the flask place 10 g. of aniline, 100 ml. of water and 10 ml. of concentrated hydrochloric acid shake until the aniline has dissolved and dilute with 400 ml. of water. 

In a 500 ml. bolt-head flask, provided with a mechanical stirrer, place 70 ml. of oleum (20 per cent. SO3) and heat it in an oil bath to 70°. By means of a separatory funnel, supported so that the stem is just above the surface of the acid, introduce 41 g. (34 ml.) of nitrobenzene slowly and at such a rate that the temperature of the well-stirred mixture does not rise above 100-105°. When all the nitrobenzene has been introduced, continue the heating at 110-115° for 30 minutes. Remove a test portion and add it to the excess of water. If the odour of nitrobenzene is still apparent, add a further 10 ml. of fuming sulphuric acid, and heat at 110-115° for 15 minutes the reaction mixture should then be free from nitrobenzene. Allow the mixture to cool and pour it with good mechanical stirring on to 200 g. of finely-crushed ice contained in a beaker. AU the nitrobenzenesulphonic acid passes into solution if a little sulphone is present, remove this by filtration. Stir the solution mechanically and add 70 g. of sodium chloride in small portions the sodium salt of m-nitro-benzenesulphonic acid separates as a pasty mass. Continue the stirring for about 30 minutes, allow to stand overnight, filter and press the cake well. The latter will retain sufficient acid to render unnecessary the addition of acid in the subsequent reduction with iron. Spread upon filter paper to dry partially. 

Place 84 g. of iron filings and 340 ml. of water in a 1 - 5 or 2-litre bolt-head flask equipped with a mechanical stirrer. Heat the mixture to boiling, stir mechanically, and add the sodium m-nitrobenzenesulphonate in small portions during 1 hour. After each addition the mixture foams extensively a wet cloth should be applied to the neck of the flask if the mixture tends to froth over the sides. Replace from time to time the water which has evaporated so that the volume is approximately constant. When all the sodium salt has been introduced, boU the mixture for 20 minutes. Place a small drop of the suspension upon filter paper and observe the colour of the spot it should be a pale brown but not deep brown or deep yellow. If it is not appreciably coloured, add anhydrous sodium carbonate cautiously, stirring the mixture, until red litmus paper is turned blue and a test drop upon filter paper is not blackened by sodium sulphide solution. Filter at the pump and wash well with hot water. Concentrate the filtrate to about 200 ml., acidify with concentrated hydrochloric acid to Congo red, and allow to cool. Filter off the metanilic acid and dry upon filter paper. A further small quantity may be obtained by concentrating the mother liquid. The yield is 55 g. 

Dissolve 10 g. of sym.-tribromoaniline (Section IV,47) in 60 ml. of rectified spirit and 15 ml. of benzene in a 200 ml. bolt-head flask by heat ing on a water bath. Add, from a burette or small graduated pipette, 5-3 g. (3-5 ml.) of concentrated sulphuric acid to the hot solution and gently swirl the liquid. Attach a reflux condenser to the flask and heat on a water bath until the clear solution boils. Detach the condenser, remove the flask from the water bath, and add 3 5 g. of powdered sodium... 

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