Aluminum hydroxide reaction with hydrochloric acid

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). 

Anhydrous aluminum chloride is currently mainly manufactured by chlorination of liquid aluminum in ceramic-lined reaction vessels at 600 to 750°C, gaseous aluminum chloride being fed into condensation chambers. The reductive chlorination of aluminum oxide in the presence of coal (e.g. in the Alcoa process, see Section 3.2.3.2) is also operated industrially. Hydrated aluminum chloride is manufactured by reacting aluminum hydroxide with hydrochloric acid or hydrogen chloride. 

The reaction of polyhydroxy bases with less than stoichiometric amounts of acids forms basic salts, that is, salts that contain unreacted OH groups. For example, the reaction of aluminum hydroxide with hydrochloric acid can produce two different basic salts ... 

For working up, the reaction mixture is poured on crushed ice and acidified with hydrochloric acid — until all the aluminum hydroxide has dissolved or the reaction mixture may be poured into a mixture of fuming hydrochloric acid and ice, best contained in a wide-neckqd separatory funnel. Adding ice and hydrochloric acid to the reaction mixture may cause local overheating and decomposition when, however, this procedure is unavoidable because of... 

This is the same equation as for the reaction of solid aluminum hydroxide with hydrochloric acid. The chloride and nitrate ions are spectators in the two reactions. 

Write a net ionic equation to represent the reaction of (a) aqueous strontium hydroxide with nitric acid (b) solid aluminum hydroxide with hydrochloric acid. 

The 2,3-dichlorophenoxyacetic acid and n-butyryl chloride are placed in the reaction vessel and stirred while the aluminum chloride is added portionwise over a 45-minute period. The mixture then is heated on the steam bath for 3 hours and allowed to cool to room temperature. The gummy product obtained is added to a mixture of 300 ml of crushed ice and 30 ml concentrated hydrochloric acid. The resulting mixture is extracted with ether and the extract evaporated at reduced pressure. The residue Is suspended in boiling water and dissolved by addition of a minimum quantity of 40% sodium hydroxide. After treatment with decolorizing charcoal and filtering, the hot filtrate is made acid to Congo red paper and chilled in ice. 

To a flame-dried, three-neck, 1-1 flask were added, in order, p-xylene (107 g, 1.0 mol), phosphorus trichloride (412 g, 3.0 mol), and anhydrous aluminum chloride (160 g, 1.2 mol). The reaction mixture was slowly heated to reflux with stirring. After 2.5 h at reflux, the reaction was allowed to cool to room temperature and the volatile components distilled at reduced pressure. The residual oil was slowly added to cold water (1 1) with stirring, and a white solid formed. The solid was removed by filtration, washed with water, and air dried. The solid was suspended in water (1 1) to which was added 50% sodium hydroxide solution (90 ml) to cause dissolution. The solution was saturated with carbon dioxide and filtered through Celite . The basic solution was washed with methylene chloride (200 ml) and acidified with concentrated hydrochloric acid (200 ml). The white solid that separated was isolated by extraction with methylene chloride (3 x 250 ml). The extracts were dried over magnesium sulfate, filtered, and evaporated under reduced pressure to give the pure 2,5-dimethylbenzenephosphinic acid (99 g, 60%) as an oil, which slowly crystallized to a solid of mp 77-79°C. 

Later, it was also claimed that 3-(tetrazolyl)-4//-pyrido[ 1,2-u]pyrimidin-4-ones 159 were obtained in an one-step procedure by heating the appropriate 2-aminopyridine, ethyl (l//-tetrazol-5-yl)acetate, and triethyl orthoformate in dimethylformamide at 90°C for 1 hour, or in boiling tetra-hydrofuran for 6 hours followed by treatment with 1N potassium hydroxide at 50°C for 1 hour, or with anhydrous aluminum chloride under reflux for 6 hours (91EUP462834). 9-Methyl-3-( 1 //-tetrazolyl)-4//-pyrido[ 1,2-a]-pyrimidin-4-one 159 (R = 9-Me) could be prepared when 2-amino-3-meth-ylpyridine hydrochloride and sodium azide were suspended and stirred in dimethylformamide for 1 hour at room temperature, followed by the addition of ethyl ethoxymethylenecyanoacetate, ethoxymethylenemalo-nonitrile, ethyl cyanoacetate and triethyl orthoformate, or malononitrile and triethyl orthoformate and stirring at 90°C for 6-12 hours. Then the reaction mixture was treated with 1 N potassium hydroxide at 50°C for 1 hour, phosphoryl chloride at 90°C for 5 hours, or with concentrated hydrochloric acid at 110°C for 4 hours to give 26-62% yields. 

The combined benzene extracts were dried and evaporated to dryness under reduced pressure to give p-butyramidophenyl acetate (38 g) as an off-white solid, MP 102-103°C. A mixture of p-butyramidophenyl acetate (38 g), aluminum chloride (80 g) and 1,1,2,2-tetrachloroethane (250 ml) was heated at 140°C for 3 hours. The reaction mixture was cooled and treated with iced water. The tetrachloroethane layer was separated and the aqueous layer was extracted with chloroform. The combined organic layers were extracted with 2 N aqueous sodium hydroxide and the alkaline solution was acidified to pH 5 with concentrated hydrochloric acid. The acidified solution was extracted with chloroform and the chloroform extract was dried and concentrated under reduced pressure to give 5 -butyramido-2 -hydroxyacetophenone (15.6 g), MP 114-117°C. A solution of 5 -butyramido-2 -hydroxyacetophenone (15.6 g) in... 

A mixture of 59.5 g (0.2 mol) 2-(4-methoxybenzyl)-l,3,3-trimethyl-4-piperidone hydrochloride and 53.8 g (0.4 mol) of aluminum trichloride and 54.0 g of nitrobenzene in 1500 ml of dry benzene are boiled under reflux for 1 h. After cooling the reaction mixture is extracted with 750 ml 4 N sodium hydroxide solution, the temperature being maintained below 35°C. The organic phase is separated and extracted with 750 ml 1 N hydrochloric acid. The acid aequeous phase is rendered alkali by the addition of 100 ml 25% ammonia and extracted three times with 250 ml chloroform. The collected chloroformic phases are dried with sodium sulfate and evaporated under reduced pressure. The residue, 46.7 g, is converted into the hydrochloride by reaction with iso-propanol/HCI and crystallized from a mixture of methanol and ethylacetate. 44.6 g of the 5-hydroxy-2 -methoxy-2,9,9-trimethyl-6,7-benzomorphan hydrochloride are obtained, melting point 233-236° C (dec.). 

In a 2-1. beaker resting on a hot plate and equipped with a mechanical stirrer are placed 150 g. of sodium hydroxide (Note 1) dissolved in 800 ml. of water and 41.4 g. (0.3 mole) of furyl-acrylic acid.1 The stirrer is started, and to the warm solution (Note 2) 100 g. of Raney nickel-aluminum alloy is added, in small portions, over a period of 4 4.5 hours (Notes 3 and 4). During the addition of the alloy, the temperature of the mixture is kept at 60-70° and then is raised to approximately 95° where it is held for an additional 2-3 hours, with stirring. From time to time sufficient water is added to the reaction mixture to maintain approximately the original volume. The hot solution is filtered by decantation, and the nickel residue (Note 5) is washed with two 50-ml. portions of hot 2% sodium hydroxide solution. The combined filtrates and washings are cooled and then immediately added slowly (Note 6), with good stirring, to 800 ml. of concentrated hydrochloric acid (Note 7). The solution at this point... 

N-4 Raney Ni.58 In a 10-ml conical flask are placed 0.5 g of Raney Ni-Al alloy powder (40% Ni) and 1 g of the bayerite prepared by the procedure described below. To this 10 ml of distilled water is added and stirred well at 40°C. Then 0.03 ml of 20% sodium hydroxide solution is added and the mixture stirred for 30 min at the same temperature, in which a violent reaction almost subsides. A further 0.3 ml of 20% sodium hydroxide solution is added and the mixture stirred for 1 h at 40°C. Then the upper layer is decanted carefully to avoid leakage of the catalyst. The catalyst is washed 3 times with each 10 ml of distilled water and 3 times with the same volume of methanol or ethanol. A specimen of the catalyst thus prepared contains 0.192 g of nickel, 0.050 g of aluminum, and 0.036 g of acid-insoluble materials. The bayerite suspensions are combined and acidified with a dilute hydrochloric acid, and then warmed to 50-60°C, when the gray color of the bayerite turns almost white. The bayerite is collected, washed well with water, and then dried in vacuo over silica gel. The bayerite thus recovered amounts to 1.4-1.6 g and can be reused for the preparation of a new catalyst. 

A mixture of 30 g. (0.16 mole) of a-naphthoyl chloride (p. 209) [Org. Syntheses Coll. Vol. 2, 425 (1943)], 30 g. (0.19 mole) of 8-methylnaphthalene, and 100 g. of carbon disulfide is cooled in an ice bath and 30 g. (0.22 mole) of powdered aluminum chloride is added slowly in small portions. The reaction mixture is stirred for 3 hours while protected from atmospheric moisture with a calcium chloride tube. The carbon disulfide is decanted from the red-brown residue, and the residue is decomposed by the gradual addition of ice and hydrochloric acid. The resulting mixture plus the carbon disulfide layer is steam-distilled to remove unreacted -methylnaphthalene. The aqueous layer is decanted from the residue in the steam distillation vessel, and the residue is treated with dilute sodium hydroxide solution. The solid remaining is washed with water and dried. The yield of crude 2-methyl-l,T-dinaphthyl ketone is 90%. Pure ketone, m.p. 140-141°, may be obtained by several recrystallizations from ethanol including activated carbon treatment. 

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