Preparation of Hydrochloric Acid

Preparation of Hydrochloric Acid with an Azeotropic Composition perform the experiment in a fume cupboard). Assemble an apparatus as shown in Fig. 20 with a few alterations. Take a conical or flat-bottomed flask without a stopper as the receiver. Fill the cooler with water. Feed the water upward through the cooler (why ). Prepare (draw out) 8-10 glass capillaries 10-12 mm long and seal them at one end. Measure the density of the initial hydrochloric acid... 

Why cannot hydrobromic acid be prepared from potassium bromide by a method analogous to that used in the preparation of hydrochloric acid ... 

It is also important in the production of aluminum (see Section 20.7). Hydrogen chloride is used in the preparation of hydrochloric acid, inorganic chlorides, and in various metallurgical processes. Hydrogen bromide and hydrogen iodide do not have any major indusUial uses. 

Immediately empty the generator into the bottle provided for the purpose. (1) Write the equation for the reaction which took place in the generator. (2) For the reaction which would have taken place at a higher temperature. (3) To what class of reactions does this preparation of hydrochloric acid belong ... 

Libavius was the first to describe the preparation of hydrochloric acid, of tin tetrachloride, and of ammonium sulfate. He described also the preparation of aqua regia ( royal water ), a mixture of nitric acid and hydrochloric acid which receives its name from the fact that it can dissolve gold. He... 

Colourless crystals m.p. 50 C, b.p. 301 C. Basic and forms sparingly soluble salts with mineral acids. Prepared by the reduction of 1-nitronaphthalene with iron and a trace of hydrochloric acid or by the action of ammonia upon l-naphlhol at a high temperature and pressure. 

The experimental conditions necessary for the preparation of a solution of a diazonium salt, diazotisation of a primary amine, are as follows. The amine is dissolved in a suitable volume of water containing 2 5-3 equivalents of hydrochloric acid (or of sulphuric acid) by the application of heat if necessary, and the solution is cooled in ice when the amine hydrochloride (or sulphate) usually crystallises. The temperature is maintained at 0-5°, an aqueous solution of sodium nitrite is added portion-wise until, after allowing 3-4 minutes for reaction, the solution gives an immediate positive test for excess of nitrous acid with an external indicator—moist potassium iodide - starch paper f ... 

Attention has previously (see Diazonium Sails) been drawn to the fact that unless an excess of hydrochloric (or mineral) acid is used in the diazotisation process, coupling occurs between the diazonium salt and the amine to give diazoamino compounds. Thus phenyldiazonium chloride and aniline yield diazoaminobenzene. This substance may be conveniently prepared by dissolving two equivalents of aniline in three equivalents of hydrochloric acid, and adding one equivalent of sodium nitrite in aqueous solution followed by two equivalents of sodium acetate ... 

This product is sufficiently pure for the preparation of phenylacetic acid and its ethyl ester, but it contains some benzyl tso-cyanide and usually develops an appreciable colour on standing. The following procedure removes the iso-cyanide and gives a stable water-white compound. Shake the once-distilled benzyl cyanide vigorously for 5 minutes with an equal volume of warm (60°) 60 per cent, sulphuric acid (prepared by adding 55 ml. of concentrated sulphuric acid to 100 ml. of water). Separate the benzyl cyanide, wash it with an equal volume of sa+urated sodium bicarbonate solution and then with an equal volume of half-saturated sodium chloride solution- Dry with anhydrous magnesium sulphate and distil under reduced pressure. The loss in washing is very small (compare n-Butyl Cyanide, Section 111,113, in which concentrated hydrochloric acid is employed). 

The class of compounds identified as basic aluminum chlorides [1327-41 -9] is used primarily ia deoderant, antiperspirant, and fungicidal preparations. They have the formula Al2(OH)g where x = 1 5, and are prepared by the reaction of an excess of aluminum with 5—15% hydrochloric acid at a temperature of 67—97°C (18). The same compounds are obtained by hydro1y2ing aluminum alkoxides with hydrochloric acid (19,20) (see Alkoxides, METAl). Basic aluminum chloride has also been prepared by the reaction of an equivalent or less of hydrochloric acid with aluminum hydroxide at 117—980 kPa (17—143 psi) (20). 

The aryl compounds are unstable substances which decompose on standing and are hydrolyzed ia moist air. The chlorides are readily prepared by the actioa of hydrochloric acid oa the corresponding arylstibonic acids. Tetraacetatopheaylantimoay [116122-86-27], C24H2yOgSb, has beea prepared (168) ... 

Arsenic pentasulfide (arsenic(V) sulfide), As S q, is stable in air up to 95°C, but at higher temperatures begins to dissociate into arsenous sulfide and sulfur. It is prepared by the fusion of arsenic with sulfur foUowed by extraction with ammonia and reprecipitation at low temperatures by addition of hydrochloric acid. Arsenic pentasulfide is precipitated at low temperatures from strongly acidic arsenate solutions by a rapid stream of hydrogen sulfide. It is hydrolyzed by boiling with water, yielding arsenous acid and sulfur. Salts derived from a number of thioarsenic acids are formed from arsenic pentasulfide and alkaH metal sulfides. 

Cobalt(II) chloride hexahydrate [7791-13-1], C0CI2 6H20 is a deep red monoclinic crystalline material that deflquesces. It is prepared by reaction of hydrochloric acid with the metal, simple oxide, mixed valence oxides, carbonate, or hydroxide. A high purity cobalt chloride has also been prepared electrolyticaHy (4). The chloride is very soluble in water and alcohols. The dehydration of the hexahydrate occurs stepwise ... 

The only practical method for preparing alkylene thioureas is by the action of the diamines upon carbon disulfide in aqueous alcohol. The final heating is essential to convert the thio-carbamic acid into the cyclic compound, the addition of hydrochloric acid being beneficial. ... 

For many years a major route to the production of vinyl chloride was the addition of hydrochloric acid to acetylene (Figure 12.5). The acetylene is usually prepared by addition of water to calcium carbide, which itself is prepared by heating together coke and lime. To remove impurities such as water, arsine and phosphine the acetylene may be compressed to 15 Ibf/in (approx. 100 kPa), passed through a scrubbing tower and chilled to -10°C to remove some of the water present and then scrubbed with concentrated sulphuric acid. 

The quindoline 224 may be prepared by the condensation of indoxyl-2-carboxylic acid with 6-aminopiperonaldehyde in the presence of hydrochloric acid, when decarboxylation and cyclization take place. Nitric acid oxidation of 224 gave an unstable nitrodicarboxylic acid which decarboxylated readily to a nitromonocarboxylic acid formulated as 8-nitro-8-carboline-3-carboxylic acid (225). ... 

Camphene hydrochloride, Cj(,H gHCl, is prepared by passing dry hydrochloric acid into an alcoholic solution of camphene. When re-ctystallised from an alcoholic solution containing excess of hydrochloric acid, it melts at 155° (or possibly a few degrees lower).- Melting-points from 149° to 165° have been recorded for this compound, but the products examined were probably not in a state of purity. 

Limonene forms a monohydrochloride, which is a liquid, and which exists in both optically active modifications. By the action of moist hydrochloric acid on the acetic or alcoholic solution of limonene, no optically active dihydrochloride is formed, the terpene becoming inactive and dipentene dihydrochloride, C (,H,g2HCl, results. This body is prepared when limonene is mixed with half its volume of glacial acetic acid, and a current of hydrochloric acid gas is passed over (not into) the well-cooled liquid, with frequent shaking. The resulting mass is pressed on a porous plate, dissolved in alcohol, and precipitated with water. It melts sharply at 50°. 

Caryophyllene nitrosochloride, (CjgHgJjN OoCL, is obtained when a mixture of the sesquiterpene, alcohol, ethyl acetate, and ethyl nitrite is cooled in a freezing mixture, and then treated with a saturated solution of hydrochloric acid in alcohol. The reaction mass is allowed to stand on ice for an hour and is then exposed to sunlight. Thus prepared it melts at about 158° to 163°, and can be separated into two compounds, one being that of a-caryophyllene and the other that of yS-caryophyllene Deussen s sesquiterpenes of natural caryophyllene from clove oil), a-caryophyllene nitrosochloride melts at 177", and /3-caryophyllene nitrosochloride at 159°. They can be separated by fractional crystallisation. The corresponding a-nitrolbenzylamine melts at 126° to 128°, and the /3-nitrolbenzylamine at 172° to 173°. The bimolecular formula given above is probable but not certain. 

Terpineol nitrosochloride, Cj Hj-OH. NOCl, is, perhaps, the most suitable derivative to prepare for the identification of terpineol. To a solution of 15 grams of terpineol in 15 c.c. of glacial acetic acid, 11 c.c. of ethyl nitrite are added. The mixture is cooled in ice, and 6 c.c. of hydrochloric acid mixed with 6 c.c. of glacial acetic acid are added drop by drop, with continual shaking. Care must be taken to avoid a rise in temperature. When the reaction is compdete, water is added to pjre-cipitate the nitrosochloride. The oily liquid soon solidifies and may be recrystallised from boiling acetic ether or from methyl alcohol. Ter-... 

Bayer and Henrich have prepared a bisnitrosopulegone, which is very useful for the identification of the ketone. A solution of 2 c.c. of pulegone in 2 c.c. of petroleum ether is cooled in a freezing mixture and 1 c.c. of amyl nitrite and a trace of hydrochloric acid are added. Fine needles of the bisnitroso compound quickly separate, which, when dried on a porous plate and washed with petroleum ether, melt at 81 5°. 

The hydrochloride is prepared by dissolving the base in the minimum amount of acetone and adding a solution of hydrochloric acid in ether until the pH is acid. The hydrochloride which has precipitated is filtered off and is recrystallized twice from acetone, melting point 116°C. 

B) Preparation of o- 2-Thienyl-(2 )-Ethyl]Benzoic Acid 24.0 g of thenylidene-(2)-phthalide, 8.8 g of red pulverized phosphorus, 240 ml of hydrochloric acid (d = 1.7) and 240 ml of glacial acetic acid are heated to boiling under nitrogen and while stirring vigorously. 70 ml toluen are then added and 6.0 g of red phosphorus added in small portions over a period of 1 hour. It is then poured into 3 liters of ice water, stirred with 300 ml of chloroform and the phosphorus removed by filtration. 

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