Mercury equipment

Any chlor-alkali plant up to modern technical standards is not a hazard to the environment. The residual emissions to water and air are ecologically acceptable according to current knowledge. The mercury in the electrolytic cells circulates in a closed system. All materials that come into contact with the mercury—equipment, products, auxiliary chemicals, wash water, waste gases, other waste materials—may... 

If preferred, the following alternative procedure may be adopted. The absolute alcohol is placed in a 1 5 or 2 litre three-necked flask equipped with a double surface reflux condenser and a mercury-sealed mechanical stirrqr the third neck is closed with a dry stopper. The sodium is introduced and, when it has reacted completely, the ester is added and the mixture is gently refluxed for 2 hours. The reflux condenser is then rapidly disconnected and arranged for downward distillation with the aid of a short still head or knee tube. The other experimental details are as above except that the mixture is stirred during the distillation bumping is thus reduced to a minimum. 

In a dry 500 ml. three-necked fiask, equipped with a mercury-sealed stirrer, a 100 ml. dropping funnel and a short fractionating column (1), place a mixture of 116 g. of anhydrous, finely-powered potassium fluoride (2) and 200 g. of dry ethylene glycol (3). Connect the fractionating... 

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... 

Pelargonic acid (n-Nonoic acid), CH3(CH2),COOH. Equip a 1-litre, three-necked flask with a reflux condenser, a mercury-sealed stirrer, a dropping funnel and a thermometer. Place 23 g. of sodium, cut in small pieces, in the flask, and add 500 ml. of anhydrous n-butyl alcohol (1) in two or three portions follow the experimental details given in Section 111,152 for the preparation of a solution of sodium ethoxide. When the sodium has reacted completely, allow the solution to cool to 70-80° and add 160 g. (152 ml.) of redistilled ethyl malonate rapidly and with stirring. Heat the solution to 80-90°, and place 182 5 g. (160 ml.) of n-heptyl bromide (compare experimental details in Section 111,37) in the dropping funnel. Add the bromide slowly at first until precipitation of sodium bromide commences, and subsequently at such a rate that the n-butyl alcohol refluxes gently. Reflux the mixture until it is neutral to moist litmus (about 1 hour). 

Into a 1500 ml. three-necked flask, equipped with a dropping funnel, a mercury-sealed stirrer and a double surface condenser (the last-named provided at its upper end with a guard tube filled witla a mixture of... 

Equip a 500 ml. three necked flask with a reflux condenser, a mercury-sealed mechanical stirrer and separator funnel, and support it on a water bath. Attach an absorption device (Fig. II, 8, 1, c) to the top of the condenser (1). Place 134 g. (152 ml.) of A.R, benzene and 127 g. of iodine in the flask, and heat the water bath to about 50° add 92 ml. of fuming nitric acid, sp. gr. 1-50, slowly from the separatory funnel during 30 minutes. Oxides of nitrogen are evolved in quantity. The temperature rises slowly without the application of heat until the mixture boils gently. When all the nitric acid has been introduced, reflux the mixture gently for 15 minutes. If iodine is still present, add more nitric acid to the warm solution until the purple colour (due to iodine) changes to brownish-red. 

Method 1 (from nitrobenzene). Support a 1 htre three-necked flask, equipped with a mercury-sealed stirrer and a reflux condenser, on a water bath, and place a solution of 65 g. of sodium hydroxide in 150 ml. of... 

Support a 1500 ml. three-necked flask, equipped with a mercury-sealed stirrer and a double surface reflux condenser, on a water bath, and place a solution of 84 g. of sodium hydroxide in 185 ml. of water, 50 g. (41-5 ml.) of nitrobenzene and 500 ml. of methyl alcohol in the flask. Add 70 g. of zinc powder (1), start the stirrer, and reflux for 10 hours. The solution gradually assumes the reddish colour of azobenzene and then on further... 

Equip a 1 Utre three-necked flask or a 1 litre bolt- head flask with a reflux condenser and a mercury-sealed stirrer. Dissolve 50-5 g. of commercial 2 4-dinitro-l-chlorobenzene in 250 ml. of rectified spirit in the flask, add the hydrazine solution, and reflux the mixture with stirring for an hour. Most of the condensation product separates during the first 10 minutes. Cool, filter with suction, and wash with 50 ml. of warm (60°) rectified spirit to remove unchanged dinitrochlorobenzene, and then with 50 ml. of hot water. The resulting 2 4-dinitrophenylhydrazine (30 g.) melts at 191-192° (decomp.), and is pure enough for most purposes. Distil oflF half the alcohol from the filtrate and thus obtain a less pure second crop (about 12 g.) recrystallise this from n-butyl alcohol (30 ml. per gram). If pure 2 4-dinitrophenylhydrazine is required, recrystallise the total yield from n-butyl alcohol or from dioxan (10 ml. per gram) this melts at 200° (decomp.). 

Equip a 500 ml, three-necked flask with a separatory funnel, a mercury-sealed mechanical stirrer and a reflux condenser. Place a solution of 21 g. of sodium hydroxide in 200 ml. of water and also 47 g. of pure phenol in the flask, and stir the mixture cool the warm mixture to about 10° by immersing the flask in an ice bath. Place 63 g. (47 ml.) of dimethyl sulphate in the separatory funnel. 

Set up the apparatus depicted in Fig. IV, 118, 1 in a fume cupboard. The narrow wide-mouthed reaction vessel A has a capacity of about 250 ml. and is equipped with a rubber stopper carrying a mercury-sealed... 

P-Hydroxy-a-naphthaldehyde, Equip a 1 litre three-necked flask with a separatory funnel, a mercury-sealed mechanical stirrer, and a long (double surface) reflux condenser. Place 50 g. of p-naphthol and 150 ml. of rectified spirit in the flask, start the stirrer, and rapidly add a solution of 100 g. of sodium hydroxide in 210 ml. of water. Heat the resulting solution to 70-80° on a water bath, and place 62 g. (42 ml.) of pure chloroform in the separatory funnel. Introduce the chloroform dropwise until reaction commences (indicated by the formation of a deep blue colour), remove the water bath, and continue the addition of the chloroform at such a rate that the mixture refluxes gently (about 1 5 hours). The sodium salt of the phenolic aldehyde separates near the end of the addition. Continue the stirring for a further 1 hour. Distil off the excess of chloroform and alcohol on a water bath use the apparatus shown in Fig. II, 41, 1, but retain the stirrer in the central aperture. Treat the residue, with stirring, dropwise with concentrated hydrochloric acid until... 

Equip a 3 litre three-necked flask with a thermometer, a mercury-sealed mechanical stirrer and a double-surface reflux condenser. It is important that all the apparatus be thoroughly dry. Place 212 g. of trimethylene dibromide (Section 111,35) and 160 g. of ethyl malonate (Section 111,153) (dried over anhydrous calcium sulphate) in the flask. By means of a separatory funnel, supported in a retort ring and fitted into the top of the condenser with a grooved cork, add with stirring a solution of 46 g. of sodium in 800 ml. of super dry ethyl alcohol (Section 11,47,5) (I) at such a rate that the temperature of the reaction mixture is maintained at 60-65° (50-60 minutes). When the addition is complete, allow the mixture to stand until the temperature falls to 50-55°, and then heat on a water bath until a few drops of the liquid when added to water are no longer alkaline to phenolphthalein (about 2 hours). Add sufficient water to dissolve the precipitate of sodium bromide, and remove the alcohol by distillation from a water bath. Arrange the flask for steam distillation (Fig. this merely involves... 

The purified commercial di-n-butyl d-tartrate, m.p. 22°, may be used. It may be prepared by using the procedure described under i o-propyl lactate (Section 111,102). Place a mixture of 75 g. of d-tartaric acid, 10 g. of Zeo-Karb 225/H, 110 g. (136 ml.) of redistilled n-butyl alcohol and 150 ml. of sodium-dried benzene in a 1-litre three-necked flask equipped with a mercury-sealed stirrer, a double surface condenser and an automatic water separator (see Fig. Ill, 126,1). Reflux the mixture with stirring for 10 hours about 21 ml. of water collect in the water separator. FUter off the ion-exchange resin at the pump and wash it with two 30-40 ml. portions of hot benzene. Wash the combined filtrate and washings with two 75 ml. portions of saturated sodium bicarbonate solution, followed by lOu ml. of water, and dry over anhydrous magnesium sulphate. Remove the benzene by distillation under reduced pressure (water pump) and finally distil the residue. Collect the di-n-butyl d-tartrate at 150°/1 5 mm. The yield is 90 g. 

Etbyl pbenylnialonate. In a I-litie flask, equipped with a dropping funnel, mercury-sealed stirrer and reflux condenser, pl oe 11-5 g. of clean sodium pieces (see Section III,7, Note I) add 250 ml. of superdry ethyl alcohol (Section 11,47,5) and allow the vigorous reaction to... 

Ethyl phenylethylmalonate. In a dry 500 ml. round-bottomed flask, fitted with a reflux condenser and guard tube, prepare a solution of sodium ethoxide from 7 0 g. of clean sodium and 150 ml. of super dry ethyl alcohol in the usual manner add 1 5 ml. of pure ethyl acetate (dried over anhydrous calcium sulphate) to the solution at 60° and maintain this temperature for 30 minutes. Meanwhile equip a 1 litre threenecked flask with a dropping funnel, a mercury-sealed mechanical stirrer and a double surface reflux condenser the apparatus must be perfectly dry and guard tubes should be inserted in the funnel and condenser respectively. Place a mixture of 74 g. of ethyl phenylmalonate and 60 g. of ethyl iodide in the flask. Heat the apparatus in a bath at 80° and add the sodium ethoxide solution, with stirring, at such a rate that a drop of the reaction mixture when mixed with a drop of phenolphthalein indieator is never more than faintly pink. The addition occupies 2-2 -5 hoius continue the stirring for a fiuther 1 hour at 80°. Allow the flask to cool, equip it for distillation under reduced pressure (water pump) and distil off the alcohol. Add 100 ml. of water to the residue in the flask and extract the ester with three 100 ml. portions of benzene. Dry the combined extracts with anhydrous magnesium sulphate, distil off the benzene at atmospheric pressure and the residue under diminished pressure. C ollect the ethyl phenylethylmalonate at 159-160°/8 mm. The yield is 72 g. 

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