Magnesium ammonium chloride

Magnesium ammonium chloride 6-hydrate can be purchased but is easily prepared by evaporation of an aqueous solution containing equimolar proportions of magnesium... 

Magaesium Chloride. Magnogene. CI2Mg mo] wt 95,23, Cl 74.46%, Mg 25.54%. MgCl2. Prepd from magnesium ammonium chloride hexahydrate in the presence of HC1 Bryce-Smith, Inorg. Syn. 6, 9 (1960). 

Other ionic species as sodium, potassium, magnesium, ammonium, chloride and sulphate were introduced as variables at constant concentrations as indicated by the groundwater analyses. These are regarded as inert species only used to guarantee a nearly correct charge balance for the ph value calculation. 

The method of hydrolysis depends on the nature of the product. It is usually sufficient to add dilute sulphuric acid to the ethereal solution and to shake thoroughly, when the magnesium enters the aqueous solution, whilst the organic compound remains in the ether. Alternatively, however, the ethereal solution may be poured on to ice and water, and then treated with dilute sulphuric acid. Should the product be affected by this acid, the hydrolysis can be carried out with an aqueous solution of ammonium chloride. In the following examples the hydrolysis is usually shown as a simple double decomposition... 

The solution was then poured into 200 ml of saturated ammonium chloride solution. After vigorous shaking the upper layer was separated off and the aqueous layer was extracted three times with diethyl ether. The combined ethereal solutions were dried over magnesium sulfate and then concentrated in a water-pump vacuum. 

To a solution of 0.40 mol of butyllithium in about 280 ml of hexane were added 280 ml of dry THF with cooling below -10°C. Subsequently 0.40 mol of 1,1-diethoxy--2-propyne (see Chapter V, Exp. 28) was introduced in 15 min at -30 to -10°C. To the solution obtained was then added in 15 min with cooling at about -15°C 0.40 mol of chloromethyl ethyl ether (note 2). After the addition stirring was continued for 1 h without cooling. The mixture was then shaken with concentrated ammonium chloride solution and the ethereal layer was separated off. The aqueous layer was extracted twice with diethyl ether. After drying the ethereal solutions over magnesium sulfate the diethyl ether was evaporated in a water-pump vacuum. 

To a solution of 22 g of K0-tert.-Ci,H9 (see Exp. 4, note 2) in 400 ml of anhydrous liquid ammonia were added 22 g of the bis-ether (note 1). After stirring for 4 h, 20 g of powdered ammonium chloride were introduced in small portions. The ammonia was removed by placing the flask in a water-bath at 40°C, then 200 ml of water were added and five extractions with small portions of redistilled pentane were carried out. The combined extracts were washed with water, dried over magnesium sulfate and then concentrated in a water-pump vacuum. The residue was carefully distilled through a 40-cm Vigreux column, giving the allenic bis-ether,... 

To a mixture of 0.20 mol of 1,1,4-triethoxy-2-butyne [see Chapter III, Exp. 40), 60 ml of dry THF and 50 ml of dry diethyl ether was added at -45 to -50°C a solution of 0.42 mol of ethyllithium in about 280 ml of diethyl ether (see Chapter II, Exp. 1). Stirring at -5o°C was continued for 30 min, then the reaction mixture was poured into 300 ml of saturated ammonium chloride solution. After shaking, the layers were separated and the aqueous layer was extracted twice with small portions of diethyl ether. The combined ethereal solutions were dried over magnesium sulfate and concentrated in a water-pump vacuum and the residue wasdistilled at about... 

To a solution of 0.40 mol of butyllithium in about 280 ml of hexane were added 300 ml of dry THF at -20 to -40 0. Subsequently 0.40 mol of freshly distilled tert.-butyl propargyl ether was added, keeping the temperature below -30°C. Freshly distilled acetaldehyde (0.40 mol) was then added at the same temperature during about 15 min. The cooling bath was removed and, after an additional 15 min, 200 ml of an aqueous solution of 30 g of ammonium chloride were introduced. After separation of the layers the aqueous layer was extracted twice with diethyl ether and the combined solutions were dried over magnesium sulfate and concentrated in... 

The aqueous layer was extracted four times with small portions of diethyl ether and the combined ethereal solutions were washed with saturated ammonium chloride solution and dried over magnesium sulfate. The greater part of the solvent was distilled... 

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