Ethyl ether absolute

In absolute ethanol solution, the ethyl ether and the corresponding hydrocarbon are formed, the latter by reduction of the diazonium compound by the ethanol, which is itself oxidised to acetaldehyde ... 

Specifications. Ethyl ether is commercially avaHable in the foHowing grades USP anesthesia, absolute (ACS), industrial, solvent (cone), and synthetic. Specifications vary, depending on the consumer and use. In many instances, the ether has to meet a specific test written into the specification, eg, it may be important that the ether is completely anhydrous or free from alcohol and aldehyde. 

Bromo-2,4-dinitrobenzene [584-48-5] M 247.0, m 75 . Crystd from ethyl ether, isopropyl ether, 80% EtOH or absolute EtOH. 

A. ot-Chloroelhyl ethyl ether. A mixture of 200 g. (201 ml.) of redistilled paraldehyde, b.p. 121-122.5° (equivalent to 4.54 moles of acetaldehyde), and 200 g. (254 ml., 4.34 moles) of absolute ethanol is placed in a 1-1. three-necked flask fitted with a mechanical stirrer and a gas inlet tube reaching to the bottom of the flask. The mixture is cooled to —5° in a mixture of Dry Ice and acetone, and dry hydrogen chloride (Note 1) is passed into the stirred reaction mixture maintained at about —5° until 200 g. (5.48 moles) has been absorbed. During this operation, which requires about 2 hours, the reaction mixture separates into two layers. The upper layer of crude a-chloroethyl ethyl ether is re-... 

The aqueous solution is then concentrated to dryness at an outside temperature of 40° to 45°C and at low pressure. The residue, obtained by drying in a vacuum at 40° to 45°C is triturated in a mortar with ethyl ether and, after filtration, is extracted with 3,400 ml boiling absolute ethanol. The ethanol extract is separated from the undissolved part by filtration, cooled and the product which crystallizes by cooling is filtered and dried at 40°C in a vacuum. In that manner the disodium (4,4 -disulfoxy-diphenyl)-(2-pyridyl)-methane bi-hydrate is obtained, which takes the form of a white solid, according to U.S. Patent 3,528,986. 

The precipitate is collected on filter paper (Note 7) in a Buchner funnel by vacuum filtration and is washed with 100 ml. of absolute ethanol. The solid is slurried in three 75-ml. portions of distilled water (Note 8), 100 ml. of absolute ethanol, two 100-ml. portions of reagent-grade acetone, and two 100-ml. portions of anhydrous ethyl ether. The filter cake is pressed dry in the funnel with suction by means of a piece of rubber dam, transferred to a tared, 500-ml., round-bottomed flask, and dried under reduced pressure (0.01 mm.) at room temperature for 24 hours (Note 9). The weight of the dry silver salt of succinimide is 51-54 g. (88-94%). 

Methylated (industrial) irit Rectified spirit (95 % CjHgOH) Ethyl alcohol (absolute) Benzene. Light petroleum (petroleum ether). ... 

Benzyltrimethylammonium chloride [56-93-9] M 185.7, m 238-239 (dec). A 60% aq soln was evapd to dryness under vac on a steam bath, and then left in a vac desiccator containing a suitable dehydrating agent. The solid residue was dissolved in a small amount of boiling absolute EtOH and pptd by adding an equal volume of ethyl ether and cooling. After washing, the ppte was dried under vac [Karusch JACS 73 1246 7957]. 

Choline chloride [67-48-1] M 139.6. Extremely deliquescent. Purity checked by AgNO3 titration or by titration of free base after passage through an anion-exchange column. Crystd from absolute EtOH, or EtOH-ethyl ether, dried under vacuum and stored in a vacuum desiccator over P2O5 or Mg(C104)2. 

Methoxyamine hydrochloride [593-56-6] M 83.5, m 151-152°. Crystd from absolute EtOH or EtOH by addition of ethyl ether. [Kovach et al. JACS 107 7360 1985],... 

Methylene Blue [61-73-4] M 319.9, 454 94,000 (EtOH), 44481,000 (HjO). Crystd from O.IM HCl (16ml7g), the crystals were separated by centrifugation, washed with chilled EtOH and ethyl ether and dried under vacuum. Crystd from 50% aqueous EtOH, washed with absolute EtOH, and dried at 50-55 for 24h. Also crystd from benzene-MeOH (3 1). Salted out with NaCl from a commercial cone aqueous soln, then crystd from water, dried at 100° in an oven for 8-1 Oh. 

A-Methyl ethylamine hydrochloride [624-60-2] M 95.6, m 126-130 . Crystd from absolute EtOH or ethyl ether. 

Methyl Violet [8004-87-3] M 394.0. Crystd from absolute EtOH by pptn with ethyl ether during cooling in an ice-bath. Filtered off and dried at 105 . 

Pinacol (anhydrous) [76-09-5] M 118.1, m 41.1°, b 172°. The hydrate is rendered anhydrous by azeotropic distn of water with benzene. Recrystd from benzene or toluene/pet ether, absolute EtOH or dry ethyl ether. Recrystn from water gives the hexahydrate. 

Thioacetamide [62-55-5] M 75.1, m 112-113 . Crystd from absolute ethyl ether or benzene. Dried at... 

D(+)-Glycogen [9005-79-2] M 25,000-100,000, m 270-280°(dec), [a]546 +216° (c 5, HjO). A 5% aqueous soln (charcoal) was filtered and an equal volume of EtOH was added. After standing overnight at 3° the ppte was collected by centrifugation and washed with absolute EtOH, then EtOH/ethyl ether (1 1), and ethyl ether. [Sutherland and Wosilait JBC 218 459 7956],... 

Mallinckrodt absolute ethyl ether (reagent grade) may be used without further drying. 

Thioacetamide [62-55-5] M 75.1, m 112-113°. Crystd from absolute ethyl ether or benzene. Dried at 70° in vacuum and stored over P2O5 at 0° under nitrogen. (Develops an obnoxious odour on keeping, and absorption at 269mm decreases, hence it should be freshly crystd before use). 

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