Liquid absolute alcohol

The use of a ternary mixture in the drying of a liquid (ethyl alcohol) has been described in Section 1,5 the following is an example of its application to the drying of a solid. Laevulose (fructose) is dissolved in warm absolute ethyl alcohol, benzene is added, and the mixture is fractionated. A ternary mixture, alcohol-benzene-water, b.p. 64°, distils first, and then the binary mixture, benzene-alcohol, b.p. 68-3°. The residual, dry alcoholic solution is partially distilled and the concentrated solution is allowed to crystallise the anhydrous sugar separates. 

Decamethylene glycol has been prepared by the reduction of dimethyl sebacate and diethyl sebacate with sodium and ethyl alcohol by the reduction of sebacamide with sodium and amyl alcohol and by the reduction of dimethyl sebacate with sodium and liquid ammonia in absolute alcohol. The reduction of esters with sodium and alcohol has also been applied to the preparation of many other glycols. ... 

Hydrolysis of the ester is achieved by refluxing in aqueous N or 2N NaOH solution until the insoluble ester dissolves. The solution is then cooled, and the alcohol is extracted into a suitable solvent, e.g. ether, toluene or alcohol-free chloroform. The extract is dried (CaS04, MgS04) and distilled, then fractionally distilled if liquid or recrystallised if solid. (The p-nitrobenzoic acid can be recovered by acidification of the aqueous layer.) In most cases where the alcohol to be purified can be readily extracted fi-om ethanol, the hydrolysis of the ester is best achieved with N or 2N ethanolic NaOH or 85% aqueous ethanolic N NaOH. The former is prepared by dissolving the necessary alkali in a minimum volume of water and diluting with absolute alcohol. The ethanolic solution is refluxed for one to two hours and hydrolysis is complete when an aliquot gives a clear solution on dilution with four or five times its volume of water. The bulk of the ethanol is distilled off and the residue is... 

To a solution of 1.38 g of estradiol 3-methyl ether (mp 118-119°) in 110 ml of anhydrous ether is added 140 ml of liquid ammonia followed by 1.4 g (42 eq per mole) of lithium wire in small pieces, and 10 min later 16 ml of absolute alcohol is added dropwise over a 10- to 20-min period. Occasionally frothing occurs during the last part of this addition but is easily controlled by stopping the stirrer temporarily. After removing most of the ammonia and carefully adding cold water, the product is extracted with ether, washed with Claisen alkali, water and saturated salt solution, and dried over sodium... 

Add 2 c.c. absolute alcohol to i c.c. sulphonic chloride and excess of caustic soda until alkaline warm gently for fire minutes and add more caustic soda if necessary. Cool, and extract with ether. The residual liquid consists of benzene ethyl sulphonate, CoH SOjCl + HOC Hj = CcH SOoOC H -p HCl. 

Quantitative Hydrolysis of Ethyl Benzoate -The quantitative estimation of an ester Ijy hycliolysis is conducted as follows a standaid half-normal solution of alcoholic potash is prepared by dissolving 7 grams of caustic potash m about an equal weight of water and diluting to 250 c.c. with absolute alcohol. The liquid is alloived to stand ovei night in a stoppered... 

After diluting the reaction liquid with acetone it is filtered, and the residue obtained after the evaporation of the filtrate in vacuo, and complete drying over pentoxide of phosphorus is then dissolved in absolute alcohol, and to this is added about the same volume of dry ether. 

In a 5-I. round-bottom flask, fitted with an efficient mechanical stirrer and surrounded by an ice-salt mixture, is placed a solution of 121 g. (0.5 mole) of pure dry finely-powdered benzoylperoxide (m.p. 104°) (Note 1) in about 1.51. of dry toluene. The temperature should be below —5°. A solution of sodium ethylate, prepared by dissolving 23 g. (1 mole) of sodium in 500 cc. of absolute alcohol, and cooled to o°, is introduced from a separatory funnel while the mixture is vigorously stirred. This operation should not require more than eight or ten minutes. The liquid whitens and thickens considerably on account of the formation of sodium benzoylperoxide. 

Lauryl alcohol has been prepared by the reduction of the aldehyde with zinc dust and acetic acid 1 by the reduction of esters of lauric acid with sodium and absolute alcohol 2 or with sodium, liquid ammonia, and absolute alcohol 3 by the reduction of lauramide with sodium and amyl alcohol.4 The method in the above procedure is essentially that described by Levene and Allen.5... 

At this point 20-30 g. of short glass fiber or asbestos is added and the yeast is filtered out by suction. The filtrate is concentrated to a thick syrup under diminished pressure on a water bath, care being taken to keep the temperature below 40° (Note 3). The residue (about 200 cc.) is taken up in a mixture of 400 cc. of absolute alcohol and 100 cc. of dry ether (Note 4). The precipitate formed is removed by centrifuging, the supernatant liquid is decanted, and the residue is extracted with a mixture of 200 cc. of 98.5 per cent alcohol and 100 cc. of dry... 

To a solution of 197 g. (1 mole) of bromoacetal1 in 250 ml. of absolute alcohol, cooled in a hydrogenation bomb of about 1.1-1. capacity to the temperature of a Dry Ice-acetone bath, is added approximately 300 g. (about 18 moles) of liquid ammonia (Note 1). The bomb is closed, connected with a pressure gauge, and heated at 120-130° with shaking for 12 hours. The pressure rises to about 2300 pounds. 

The liquid was then evaporated in vacuo to a small volume and two volumes of 95% ethanol were added. A small amount of flocculent precipitate, probably consisting of yeast polysaccharides, was removed by centrifugation, and the solution was concentrated to a sirup in a vacuum oven at 40°. This colorless sirup, when treated with hot absolute alcohol and stirred, set to a crystalline mass. The crystals were filtered, washed with alcohol and ether and dried in vacuo at 70°. The yield was 2.8 g. 

A mixture of acetamide (30 g. = 0-5 mole) and bromine (80 g. = 26 c.c.) in a half-litre flask is kept well cooled with water while enough of a solution of 50 g. of potassium hydroxide in 350 c.c. of water is added to change the initially red-brown colour into a pale yellow this requires most of the alkali. The solution is now run from a dropping funnel in an unbroken jet into a solution of 80 g. of potassium hydroxide in 150 c.c. of water, maintained at 70°-75° in a litre flask. The operation lasts for several minutes. Until the reaction mixture becomes colourless (one quarter to half an hour) the temperature is maintained at 70°-75°, and then the methylamine is distilled with steam. An adapter is fixed to the lower end of the condenser and dips 1 cm. below the surface of the liquid in the receiver (100 c.c. of approximately 5 N-hydrochloric acid2). As soon as the liquid which forms in the condenser is no longer alkaline the distillation is discontinued and the contents of the receiver are evaporated to dryness in a porcelain basin on the water bath. The last traces of water are removed by allowing the basin to stand over night in a vacuum desiccator. The dried material is boiled with absolute alcohol, which dissolves the methylamine hydrochloride but not the ammonium chloride with which it is mixed. The clear filtrate obtained when the ammonium chloride is removed by filtration is concentrated to a small volume and the methylamine hydrochloride is allowed to crystallise out in the cold. The salt is filtered with suction, washed with a little alcohol, and dried in a desiccator. Yield 15-20 g. 

A solution of 25 g. of sodium hydroxide in 500 c.c. of water is heated to boiling (porous pot ) in a distilling flask (capacity 1 1.) connected to a downward condenser which is provided with a receiver containing 60 c.c. of 2 A-hydrochloric acid. Through the corked neck of the flask 18-6 g. of nitrosodimethylaniline hydrochloride—preferably the moist reaction product—are added in portions. Each addition is only made after most of the oily drops of the base from the preceding portion have dissolved, and finally the liquid is boiled until it has become reddish-brown. The dimethylamine produced is trapped in the hydrochloric acid in the receiver at the conclusion of the distillation the contents of the receiver must still be acid. They are evaporated to dryness on the wateT bath in a small porcelain or glass basin, and finally the completely anhydrous salt can be recrystallised from a very small amount of absolute alcohol. Yield 5-6 g. 

The crude product contains varying quantities of sodium carbonate and sodium sulfate, which are difficult to remove. These impurities are insoluble in liquid ammonia consequently the crude compound can be ammonolyzed without further purification. The mandelic acid-acetone condensation product may be purified by recrystallization from absolute alcohol it then melts at 45°. 

Anhydrous salt is a colorless, cubic, crystalline solid refractive index 1.650 density 3.052 g/cm melts at 875°C vaporizes at 1,250°C very slightly soluble in absolute alcohol and acetone insoluble in liquid ammonia. 

Chloropicrin (PS)—trichloronitromethane, CCl3N02 Green Cross, Klop—Is a colorless, volatile, slightly oily liquid with an Intense odor (see Table 4-1). It is very slightly soluble in water, soluble in ether, and miscible with benzene, absolute alcohol, and carbon disulfide.10It boils at about 112°C. 

Thallous halides do not absorb ammonia at ordinary temperature, but in liquid ammonia these salts form triannnino-thallous halides of composition [T1(NH3)3]C1, [Tl(NH3)3]Br.1 The triammino-deriva-tives formed are somewhat soluble in liquid ammonia, and the solubility increases with rise of temperature and increase in atomic weight of the halogens. No lower ammino-derivatives are known. Tliallic halides absorb ammonia gas readily. If ammonia gas is passed into an alcoholic solution of thallic chloride, or if dry ammonia gas is passed over dry thallic chloride, the gas is absorbed and a white crystalline substance is formed of composition [T1(NH3)3]C13. The crystals may be washed with alcohol containing ammonia and then with absolute alcohol, and finally dried in vacuo. On coming in contact with water the triammine is decomposed with precipitation of violet-black oxide thus ... 

Ethyl alcohol, also called ethanol, absolute alcohol, or grain alcohol, is a clear, colorless, flammable liquid with a pleasant odor. It is associated primarily with alcoholic beverages, but it has numerous uses in the chemical industry. The word alcohol is derived from the Arabic word al kuhul, which was a fine powder of the element antimony used as a cosmetic. In Medieval times, the word al kuhul came to be associated with the distilled products known as alcohols. The hydroxyl group, -OH, bonded to a carbon, characterizes alcohols. Ethyl is derived from the root of the two-carbon hydrocarbon ethane. 

A mixture of 150 parts of oxalic acid, 40 of potassium chlorate, and 20 of water is heated to 60°, and the soln. cone, in vacuo at 50° until it begins to crystallize. The cold liquid i3 then treated with 3 volumes of absolute alcohol, when potassium carbonate is precipitated. Fine deliquescent needles of potassium chlorite can be obtained by fractional crystallization in vacuo. The residue gives a further crop of crystals of the chlorite by treatment with 95 per cent, alcohol. Small yellow crystals of silver or lead chlorites can be obtained by double decomposition. 

A soln. of 20 grms. of potassium iodide, in a small proportion of water, is poured into a hot soln. of 40 grms. of potassium permanganate in a litre of water. The mixture is heated on a water bath for about half-an-hour, and alcohol is added, drop by drop, to the pink soln. until the permanganate is decolorized. Filter the mixture, and wash the precipitate which is probably potassium manganite. Just acidify the alkaline filtrate with acetic acid, and evaporate the liquid down to about 50 o.o. The mother liquor is poured from the granular crystals of potassium iodate which separate as the soln. cools, the crystals are washed repeatedly with absolute alcohol, and dried. About 25 grms. of potassium iodate are so obtained. 

Lithium.—In order to extract lithium from the silicate minerals—petalite, lepidolite, spodumene, amblygonite, etc.—J. J. Berzelius 3 fused the finely powdered mineral with twice its weight of calcium or barium carbonate. L. Troost fused a mixture of finely powdered lepidolite with an equal weight of barium carbonate, half its weight of barium sulphate, and one-third its weight of potassium sulphate. In the latter case, two layers were formed lithium and potassium sulphates accumulated in the upper layer from which they were extracted by simple lixiviation. The sulphates are converted to chlorides by treatment with barium chloride. The filtered liquid is evaporated to dryness, and the chlorides extracted with a mixture of absolute alcohol, or pyridine. The lithium chloride dissolves, the other alkali chlorides remain as an almost insoluble residue. 

Precipitate with aq. ammonia. Evaporate the soln. down to about 100 c.c., and filter the ot liquid so as to remove calcium sulphate. The cone. soln. is sat. with ammonium alum and allowed to stand for some time. The mixed crystals of potassium, rubidium, and oeesium alums and of lithium salt are dissolved in 100 c.c. of distilled water and recrystal-lized. The recrystallization is repeated until the crystals show no spectroscopic reaction for potassium or lithium. The yield naturally depends on the variety of lepidolite employed. 100. grms of an average sample gives about 10 grms. of crude crystals and about 3 grms. of the purified caesium and rubidium alums. For the purification of caesium and rubidium salts, see the chlorides. The mother-liquors are treated with an excess of barium carbonate, boiled, and filtered. The filtrate is acidified with hydrochloric acid, and evaporated to dryness. The residue is extracted with absolute alcohol in which lithium chloride is soluble, and the other alkali chlorides are sparingly soluble. 

The so-called potassium or sodium hydroxide pure by alcohol 20—e.g. soude a I alcool—was prepared by C. L. Berthollet in 1786 by dissolving the hydroxide in absolute alcohol. Most of the impurities remain undissolved, but a little chloride, carbonate, and acetate pass into the alcoholic soln. The alcoholic soln. is allowed to settle, the clear liquid is decanted off, and evaporated in a silver dish, on a water-bath. The resinous matter which is formed, is removed from the warm semi-solid mass by means of a silver spatula, and the mass is then poured on a plate of polished iron. 

For preparing larger quantities of the hydrosulphide it is more convenient to carry out the reaction in the presence of an excess of the precipitant—say 5 grins, of sodium with a mixture of 10 grms. of absolute alcohol and 100 c.c. of pure dry benzene, more alcohol is added from time to time to keep the ethoxide in soln. until all the sodium is dissolved. This liquid is treated with hydrogen sulphide as before. The reaction seems to be quantitative and to be expressed by the equation C2H50Na+H28=C2H50H+NaHS potassium salt is prepared in a similar manner. 

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