Color ethyl ether

The solution in the left flask is stirred for 30 minutes after all the potassium amide has been added. The nitrogen inlet is briefly removed and 120 g. (1.5 moles) of ammonium nitrate is added this discharges the ehartreuse color. (Caution Vigorous foaming occurs.) Ethyl ether (500 ml.) is added and the dry iee condenser is replaced by a standard water-cooled condenser. I he ammonia is evaporated by allowing the stirred reaction mixture to warm to room temperature this takes several hours iti(l it is convenient to have it occur overnight. 

Chemical Designations - Synonyms Cellosolve Dowanol EE 2-Ethoxyethanol Ethylene Glycol Ethyl Ether Glycol Monoethyl ether Poli-Solv EE Chemical Formula HOCHjCH OCHjCHj. Observable Characteristics - Physical State (as shipped) Liquid Color Colorless Odor Sweetish mild, pleasant, ethereal. 

Upon completion of the addition, the mixture is agitated for 7 hours at ambient temperature. The solution is then poured into 3 liters of water/ice obtaining a clear solution of dark yellow color which is rendered alkaline upon phenolphthalein with 30% NaOH and extracted with ethyl ether to eliminate the majority of the pyridine. The mixture is filtered with active charcoal, the pH adjusted to 8 with hydrochloric acid 1 1 and extracted with chloroform to remove the 4,4 -dihydroxydiphenyl-(2-pyridyl)-methane which has not reacted. 

A suspension of sodium amide2 (0.1 mole) in liquid ammonia is prepared in a 500-ml. three-necked, round-bottomed flask fitted with a West condenser, a ball and socket glass mechanical stirrer (Note 1), and a dropping funnel. In the preparation of this reagent a small piece of clean sodium metal is added to 350 ml. of commercial anhydrous liquid ammonia. After the appearance of a blue color, a few crystals of hydrated ferric nitrate are added, whereupon the blue color is discharged. The remainder of the 2.3 g. (0.1 mole) of sodium (Note 2) is then rapidly added as small pieces. After all the sodium has been converted to sodium amide (Note 3), a solution of 16.4 g. (0.1 mole) of ethyl phenyl-acetate (Note 4) in 35 ml. of anhydrous ethyl ether is added dropwise over a 2-minute period, and the mixture is stirred for 20 minutes. To the dark green suspension is added over an 8-minute period a solution of 18.5 g. (0.1 mole) of (2-bromo-... 

The product is pale yellow. The color may be removed by crystallizing the material from a mixture of 100 cc. of petroleum ether and about 10 cc. of ethyl ether. The recovery is 21 g. (91 per cent). 

Tellurium O-ethylisobutyrylacetone trichloride (Formula I).— Tellurium tetrachloride (1 mol.) is heated with isobutyrylacetone (B.pt. 95° C.) (2 mols.) in chloroform solution for one hour, the reaction mixture filtered from free tellurium and evaporated in a vacuum. The trichloride thus obtained in about 30 per cent, yield crystallises from benzene-petroleum mixture as pale yellow flakes or needles, M.pt. 103° C. with decomposition. It gives no coloration with ferric chloride, and is decomposed by 5N sodium hydroxide, the odour of the O-ethyl ether of the j8-diketone being noticed. 

Solvent extraction Immediately after preparation, the browning product mixture was continuously extracted first with light petroleum, b.p. 60-80, and then with ethyl ether. About 2 h were required for each stage before no further color was extracted. In each case the solvent was removed under vacuum 4. 60°. 

A suspension of bromobis[2,3-butanedione dioximato( 1 -)] (4-rerr-butylpyri-dine)cobalt(III) (2.5 g, 5.0 mmole) (see above) in 20 mL of methanol in a 100 mL, three-necked flask is vigorously stirred under an N2 purge for 10 minutes. While it is stirred and purged with N2, solid sodium tetrahydroborate (0.5 g, 13 mmole) is gradually added in about 0.1-g portions. Upon addition of the sodium tetrahydroborate, the solution becomes warm, shows considerable effervescence due to hydrogen evolution, and becomes homogeneous. The development of the dark blue-black color is characteristic of the reduced Co(I) species. Then 2-bromoethyl ethyl ether (0.56 mL, 5.0 mmole) is added and the solution turns red-brown, indicating the presence of the alkylcobalt(III) species. The reaction mixture is then stirred for 15 minutes. To obtain maximum yields, another 0.25 g of solid sodium tetrahydroborate is added, followed by addition of an extra 0.25 mL of 2-bromoethyl ethyl ether. The reaction mixture is stirred for another 10 minutes. Further additions of sodium tetrahydroborate and 2-bromo-... 

The sample used must have a negative hexabromide test, indicating the absence of acids more highly unsaturated than linoleic. The test is carried out as follows 2 cc. of the oil and 25 cc. of a 4 1 ethyl ether-glacial acetic acid mixture are chilled to 0° for fifteen to twenty minutes the mixture is filtered if it is not clear. To this solution is added sufficient bromine to give a deep red color, and the whole is allowed to stand for fifteen minutes. The absence of a precipitate constitutes a negative test. 

B) Hexabromostearic Acid.—In a 4-1. beaker equipped with a mechanical stirrer (Note 1), 90 to 95 g. of the fatty acids is dissolved in 2.5 1. of ethyl ether, and the solution is chilled to 0-10°. Then, with stirring, 35 cc. of bromine (Notes 2 and 3) is introduced slowly, from a dropping funnel (Note 4), at such a rate that the temperature does not exceed 20° about fifty minutes is usually required. The solution, which must contain an excess of bromine (deep red color), is allowed to stand in an ice bath at 0-10° overnight. The excess bromine is removed by addition of a small amount of amylene, and then the white precipitate is collected with suction on a 12.5-cm. Buchner funnel and is washed with 200 cc. of ethyl ether. The hexabromide is... 

The receiver containing the ethereal solution of trimethyl-stibine is kept in ice, and the stopper is replaced with a gas inlet tube connected to a cylinder of chlorine. The inlet tube should extend at least 2 cm. below the level of the liquid in the flask. The mixture is stirred slowly and chlorine is bubbled in until the slurry turns yellowish in color. The precipitate of trimethylantimony dichloride which has formed during the chlorination is removed by filtration on a fritted Buchner funnel and washed several times with ethyl ether. The yield of crude product is 95.9 g. (64.2% of theoretical based upon SbCls). 

The preparation of trimethylantimony diiodide is identical to that of trimethylantimony dichloride up to the point of the addition of chlorine. Instead of a gas inlet tube, an addition funnel is mounted on the flask containing the ice-cold distillate of ethyl ether and trimethylstibine. For a reaction carried out on the basis of 0.25 mol of anhydrous antimony(III) chloride, a solution of 63,5 g. (0.25 mol) of iodine in 400 ml. of ethyl ether is prepared. This solution is added dropwise to the cold distillate. Stirring is maintained and the addition is continued until the color of iodine persists. The precipitate of trimethylantimony diiodide is filtered off on a fritted Buchner fuimel and washed with ethyl ether. The jdeld of the crude product is 47.7 to 65.3 g. (45.0 to 61.8% of theoretical based upon antimony (III) chloride). The diiodide may be recrystallized from ethanol. Anal. Calcd. for (CH3) 3Sbl2 Sb, 28.95 C, 8.55 H, 2.16. Found Sb, 29.31 C, 8.16 H, 2.25. The checkers report that the foregoing syntheses are also satisfactory using one-half the amounts prescribed. 

Anhydrous ethanol (65 cm3 vas added to dried APS - Y zeolite (1.5 g) under a nitrogen atmosphere and the suspension was stirred for 0.5 h. Then, a solution of 2,3-butanedione (0.5 cm3) in 35 cm3 of methanol was added and the mixture was stirred at 25°C fo 24 h. The resulting modified zeolite was filtered off, washed with a mixture (1-1) of ethyl ether and dichloromethane (150 cm3) using a Soxhlet apparatus overnight and dried at 100°C. The color of the dried modified zeolite was pale yellow as the corresponding grafted silica according to [12]. 

Ethyl ether or ethyl acetate are percolated through the mixture. Acetic acid is used to extract the bases from the solvent. The acetic acid/ base solution is washed with ether until the ether absorbs no more color. The bases are precipitated with sodium carbonate, washed, dried and dissolved in ethyl ether. 

Properties Finely crystalline, light yellow color. D 0.868, bulk d 0.617, mp decomposes (often violently) 166C, pure material 167-168.5C. Soluble in methanol, ethyl ether, and hot water. 

Fig. 1 Phase diagrams of methanol mixtures with (A) ethyl ether at 115°C and (B) u-pentane at 99.6°C. (From Refs. . ) (View this art in color at WWW. dekker. com.)...

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