Magnesium bromide, anhydrous

Magnesium bromide (anhydrous) [7789-84-6] M 184.1. Crystd from EtOH. 

Magnesium bromide, anhydrous, MgBr2 [1,629, before Magnesium bromide etherate]. Mol. wt. 184.15. Supplier A. D. MacKay, Inc. 

Add 4 0 g. (4 0 ml.) of pure anihne dropwise to a cold solution of ethyl magnesium bromide (or iodide) prepared from 1 Og. of magnesium, 5 0 g. (3-5 ml.) of ethyl bromide (or the equivalent quantity of ethyl iodide), and 30 ml. of pure, sodium-dried ether. When the vigorous evolution of ethane has ceased, introduce 0 02 mol of the ester in 10 ml. of anhydrous ether, and warm the mixture on a water bath for 10 minutes cool. Add dilute hydrochloric acid to dissolve the magnesium compounds and excess of aniline. Separate the ethereal layer, dry it with anhydrous magnesium sulphate and evaporate the ether. Recrystallise the residual anihde, which is obtained in almost quantitative yield, from dilute alcohol or other suitable solvent. 

A slow stream of purified and dried acetylene is passed for 3 hr through a solution containing 25 ml (75 mmoles) of a 3 TV solution of methyl magnesium bromide and 100 ml of anhydrous tetrahydrofuran. A solution consisting of 5 g (17 mmoles) of 3)5-hydroxyandrost-5-en-17-one and 50 ml of anhydrous tetrahydrofuran is then added and the mixture is boiled at reflux for 15 min, during which time a heavy precipitate forms. The reaction mixture is cooled and poured into 1 liter of water containing 20 ml of concentrated sulfuric acid. The crude product is obtained as a precipitate, which is filtered, washed with water and dried to yield 5.2 g of 17a-ethynylandrost-5-ene-3, 17 -diol mp 228-232°. One crystallization from chloroform-hexane yields 4.5 g (83%) mp 238-240° [[Pg.73]

The formation of diphenyl on oxidation of phenyl magnesium bromide by anhydrous ferric chloride has been known for some... 

Aj Preparation of (2-Amino-5-ChlorophenyljPhenylmethaneimine (4356 CB) A solution of 228.7 g (1.5 mols) of 2-amino-5-chlorobenzonitrile in 1,800 ml of dry ether is added slowly in the course of about 3.5 hours to a solution of phenyl magnesium bromide prepared from 109 g (4.5 g-atoms) of magnesium turnings and 848 g (5.4 mols) of bromobenzene In 3,600 ml of anhydrous ether, and the mixture then heated under reflux for 15 hours. 

Preparation of 3-Hexyne-2-ol A solution of ethyl magnesium bromide was prepared by the reaction of 229 g of ethyl bromide and 4B.6 g of magnesium in 750 ml of anhydrous ether. To the ether solution was then added with stirring a solution of 10B g of ethyl acetylene in 250 ml of cold anhydrous ether. The addition required approximately 3 hours, and the mixture was stirred and refluxed for a further period of 3V2 hours. Thereafter there was added to the reaction mixture a solution of BB g of freshly distilled acetaldehyde in 170 ml of anhydrous ether, over a period of about 45 minutes and at a temperature in the range of about -10° to 0°C. 

Addition of anhydrous magnesium bromide to [l,3-bis(trimethylsilyl)-2-propenyl]lithium improves the antijsyn selectivity of the reaction with benzaldehyde from 80 20 to 94 6 23. 

Nitric acid. Sulfuric acid, N-Methylhydroxy acetamide Phosphorus oxytrichloride. Benzene, Neopentyl glycol. Pyridine, Petroleum ether. Ammonium fluoride Thiophosphorus trichloride. Benzene, Neopentyl glycol. Pyridine, Petroleum ether. Ammonium fluoride Nitric acid. Sulfuric acid. Glycerol, Magnesium sulfate Anhydrous hydrazine. Cyanogen bromide. Isopropyl alcohol. Sodium nitrite. Sodium bicarbonate. Copper nitrate trihydrate. Nitric acid. Diethyl ether... 

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