Carbonic acid mixture with magnesium hydroxide

Synonyms carbonic acid, magnesium salt (1 1), mixture with magnesium hydroxide and magnesium hydrate dypingite E504. 

Carbonic acid, magnesium salt (1 1), mixture with magnesium hydroxide (Mg(OH)2), hydrate CCRIS 7884 Magnesium carbonate basic Magnesium carbonate hydroxide Marinco C. A basic magnesium carbonate of variable composition. Used in fireprooSnp, as an antacid and laxative and in manufacture of magnesium compounds. 

The reaction mixture is then transferred to a 2-I. round-bottom flask with wide neck, and to this is added all at once 300 g. of cracked ice, and the mixture is rapidly agitated by a rotary motion until the decomposition is complete (Note 7). Sufficient 30 per cent sulfuric acid is added to dissolve the magnesium hydroxide, and the mixture is then steam-distilled until oil no longer collects on the surface of the distillate. The distillate, which amounts to 1500-2500 cc., is saturated with sodium chloride and the upper layer separated. The aqueous layer is extracted with two loo-cc. portions of ether and the ether extract added to the alcohol layer. The ether solution is dried over anhydrous potassium carbonate, filtered, and heated carefully on the steam cone until all the ether is distilled. The crude alcohol is warmed one-half hour with about 5 g. of freshly dehydrated lime (Note 8). After filtering again and washing the lime with a little ether, the ether is distilled and the alcohol is distilled in vacuo from a Claisen flask (Note g). The carbinol distils at 88-93 /18 mm. (practically all distilling at 91°). The yield is 70-74 g. (61-65 P r cent of the theoretical amount) (Note 10). 

Benzophenoneoxime has been prepared in quantity by treating an aqueous alcoholic mixture of benzophenone and hydroxyl-amine hydrochloride with hydrochloric acid,2 with sodium carbonate,3 with alcoholic potassium hydroxide,4 or with aqueous sodium hydroxide. It has also been obtained by treating bis-nitrosylbenzohydryl with alcoholic potassium hydroxide,6 and by the oxidation of a-aminodiphenylmethane with magnesium persulfate solution.7... 

A. l-Phenyl-2,2,2-lrichloroethanol. In a 1-1. round-bottomed-flask fitted with a mechanical stirrer, a thermometer, and a powder funnel is placed a solution of 212 g. (2.00 moles) of freshly distilled benzaldehyde in 400 g. (270 ml., 3.35 moles) of chloroform. The mixture is cooled in an ice bath, and 123 g. of commercial powdered potassium hydroxide is added with stirring at such a rate that the temperature of the solution does not exceed 45° (1-1.5 hours). The reaction mixture is stirred and kept at 40-50° for an additional hour and then poured into a solution of 60 ml. of sulfuric acid in 3 1. of water. The resulting two-phase mixture is transferred to a separatory funnel and extracted with three 250-ml. portions of chloroform (a small amount of insoluble, black resinous material is discarded). The combined organic layers are washed with three 100-ml. portions of aqueous 10% sodium carbonate, dried over anhydrous magnesium sulfate, and filtered into a 1-1. flask. The solvent is removed under reduced pressure on a hot water bath. The residue is transferred to a 250-ml. flask and distilled under reduced pressure to give l-phenyl-2,2,2-trichloroethanol, b.p. 155-165° (26 mm.), 90-100° (0.5 mm.) (Notes 1 and 2). The yield is 170-180 g. (38-40%). 

Method B. Dissolve 55.2 g (0.32 mol) of pure decanoic acid, m.p. 31-32°C, and 25.6 g (0.16 mol) of methyl hydrogen adipate in 200 ml of absolute methanol to which 0.25 g of sodium has been added. Electrolyse at 2.0 amps at 25-35 °C until the pH of the electrolyte is 8.2 (c. 9 hours). Neutralise the contents of the electrolytic cell with acetic acid, distil off the methanol on a water bath, dissolve the residue in about 200 ml of ether, wash with three 50 ml portions of saturated sodium hydrogen carbonate solution and remove the ether on a water bath. Treat the residue with a solution of 8.0 g of sodium hydroxide in 200 ml of 80 per cent methanol, reflux for 2 hours and distil off the methanol on a water bath. Add about 600 ml of water to the residue to dissolve the mixture of sodium salts extract the hydrocarbon with four 50 ml portions of ether, and dry the combined ethereal extracts with magnesium sulphate. After removal of the ether, 23.1 g of almost pure octadecane, m.p. 23-24 °C, remains. Acidify the aqueous solution with concentrated hydrochloric acid (c. 25 ml), cool to 0 °C, filter off the mixture of acids, wash well with cold water and dry in a vacuum desiccator. The yield of the mixture of sebacic and myr-istic acids, m.p. 52-67 °C, is 26 g. Separate the mixture by extraction with six 50 ml portions of almost boiling light petroleum, b.p. 40-60 °C. The residue (5.2 g), m.p. 132°C, is sebacic acid. Evaporation of the solvent gives 20 g (55%) of myristic acid, m.p. 52-53 °C the m.p. is raised slightly upon recrystallisation from methanol. 

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