Ethyl acetic acid ether

Ethyl acetic acid ether was treated with hydroxylamine and acetohydroxamic acid was obtained. 

The foUowing are typical experimental details for the preparation of naphthalene picrate. Dissolve 0 -1 g. of naphthalene and 0-2 g. of picric acid separately in the minimum volume of hot rectified spirit (about 2 ml.), mix the solutions and allow to cool. FUter and wash with 2 ml. of alcohol. RecrystaUise from hot alcohol, ethyl acetate or ether. 

To obtain crystalline perbenzoic acid, dry the moist chloroform solution with a little anhydrous sodium or magnesium sulphate for an hour, filter, and wash the desiccant with a little dry chloroform. Remove the chloroform under reduced pressure at the ordinary temperature whilst carbon dioxide is introduced through a capillary tube. Dry the white or pale yellow residue for several hours at 30-35° under 10 mm. pressure. The yield of crystalline perbenzoic acid, m.p. about 42°, which is contaminated with a little benzoic acid, is 22 g. It is moderately stable when kept in the dark in a cold place it is very soluble in chloroform, ethyl acetate and ether, but only shghtly soluble in cold water and in cold hght petroleum. 

L-Malic acid [97-67-6] M 134.1, m 104.5-106 , [ajp -2.3 (c 8.5, HjO), pK, 3.46, pK 5.10. Crystd (charcoal) from ethyl acetate/pet ether (b 55-56°), keeping the temperature below 65°. Or, dissolved by refluxing in fifteen parts of anhydrous diethyl ether, decanted, concentrated to one-third volume and crystd at 0°, repeatedly to constant melting point. 

Bromo-4-methoxy-A-homo-estra-2,4,5(10)-trien-17-one (44 0. 2g), is dissolved in formic acid, 2 ml of boron trifluoride etherate is added and the mixture is stirred vigorously at 0° for 2 hr. A brown mass ca. 0.12 g) is obtained after evaporation of the solvents at reduced pressure. This material is diluted with water and extracted with chloroform. The chloroform extracts are washed successively with water and saturated salt solution, dried over anhydrous magnesium sulfate and evaporated at reduced pressure to give 95 mg of a product which is purified by filtration through a column of neutral alumina and crystallization of the residue after evaporation of the solvent from ethyl acetate-petroleum ether. The resulting A-homo-estra-l(10),2,4a-triene-4,17-dione (45), mp 143-146°, is identical to the tropone (45) prepared from monoadduct 17-ketone (43a). 

In a variation of this procedure that gives a nearly quantitative yield of good material, the intermediate salt is dissolved in 250 ml. of glacial acetic acid in a 2-1. beaker, and 100 g. of 50% fluoboric acid is added with stirring. When the evolution of gas has stopped, 11. of ethyl acetate is added to precipitate tropylium fluoborate. The fluoborate is separated by filtration, washed successively with ethyl acetate and ether, and dried in an oven at 40°.4... 

Eluent components should be volatile. Solvents such as ethyl acetate, isopropyl ether, diethylketone, chloroform, dichloromethane, and toluene as modifiers and n-hexane as diluent are recommended for normal phase chromatography. For reversed-phase systems, methanol or acetonitrile are used as modifiers. Such components as acetic acid or buffers, as well as ion association reagents, should be avoided. 

Solvent Beverages Acetaldehyde Acetic Acid H Hi ethyl Filter Ethyl Acetate Glycol Ether... 

A mixture of 5.54 g (40 mmol) of 3-methylpentanedioic acid, 14.8 g (80 mmol) of methyl (R)-2-thioxo-4-thi-azolidinecarboxylate, 18.16 g (88 mmol) of dicyclohexylcarbodiimide, and 100 mL of pyridine is stirred at r.t. for 6 d. After evaporation of the excess solvent in vacuum, the residue obtained is treated with 150 mL of benzene, the precipitated urea is filtered off and the filtrate is condensed in vacuum to give 50 mL of solution. Flash-chromatography on a short silica gel column with benzene/ethyl acetate (10 1) affords yellow needles yield 13.0 g (70%) mp 113-114°C (ethyl acetate/diethyl ether) [a] —163.9 (c = 1.00, ethyl acetate). 

OaN-C-C(CHs)-C-NOa (decomp) and defgr when heated to higher temps. Sol in ale, ethyl acetate and ether. Was obtained (tog ether with 3,5-din itro-p-xylene-2-diazoniumnitrate) by treating. 5-amino-p-xyIene-2-sulfonic acid with HN03 (d 1.51) at -5°- Its expl props were not investigated... 

A solution of methyl 3,6-dichloro-3,6-dideoxy-p-D-allopyranoside (25, 148 mg) in ethanol (50 mL) containing potassium hydroxide (70 mg) and W-4 Raney nickel [27,58] (40 mg) was shaken in an atmosphere of hydrogen for 2 days. A solid product was isolated in the usual manner recrystallization from ethyl acetate-petroleum ether gave methyl 3,6-dideoxy-P-D-nbo-hexopyranoside (35, 89 mg, 86%) mp 63°-65°C, [a]D —60° (c 1.5, MeOH). A solution of methyl 3,6-dideoxy-p-D-ribo-hexopyranoside (35, 86 mg) in 1 N sulfuric acid (10 mL) was heated at 90°C for 5 h. The cooled solution was neutralized with Duolite A-4(OH ) iou-exchange resin and concentrated to yield paratose 36 as a homogeneous (TLC) syrup (61 mg, 78%) R 0.21 [Silica Gel G 6 1 (v/v) chloroform-methanol], [a]D +7° (c 1.1, HzO), in agreement with values reported previously [61,62] for paratose. 

To a solution of Fmoc-Thr(Ac3GalN3)-OAll 26 (4.0 g, 5.8 mmol) in dry THF (50 mL) is added at 0°C acetic acid (1 mL) and, subsequently, a solution of tri-n-octylphosphine (3.4 mL, 7.4 mmol) in THF (10 mL). After 2 h, the mixture is concentrated in vacuo. To complete the / /-acetylation, the remainder is stirred with acetic anhydride (2 mL)-pyridine (10 mL) for 6 h, concentrated in vacuo. Toluene (3 x 20 mL) is distilled in vacuo from the residue, which is subsequently purified by flash chromatography on silica gel (100 g) in petroleum ether-ethyl acetate —> ethyl acetate. The product is recrystallized from ethyl acetate-petroleum ether yield, 3.9 g (94%) mp 66-68° C [a]D +36.3° (c 1, CHC13) Rf 0.56 (ethyl acetate). 

The solvents 1, ethyl acetate-2-propanol-water (126 70 35) 2, 2-propanol-water (90 10) 3, benzene-methanol (10 3) 4, chloroform-acetone (1 7) 5, 1-butanol-acetic acid-ether-water (0 6 3 1) 6, chloroform-2,2,4-trimethylpentane-methanol (50 15 5) 7, chloroform-methanol (10 2). 

Figure D1.6.2 TLC-FID separation of lipids recovered from the gastric contents of a hooded seal pup. The mobile phase was 91 6 3 1 (v/v/v/v) hexane/ethyl acetate/diethyl ether/formic acid. Time refers to scanning time of the Chromarod. Abbreviations DG, 1,2-diglyceride FFA, free fatty acid MG, monoglyceride IS, internal standard TG, triglyceride. Reproduced from Ackman and Heras (1997) with permission from AOCS Press.

Commonly used extraction solvents are ethyl acetate, diethyl ether, methanol, and aqueous methanol, but the majority of the free phenolic compounds can be extracted with alcohols (methanol or ethanol) or alcohol-water mixtures (1). Due to the differences in polarity between components (40), neither diethyl ether nor ethyl acetate are able to extract completely all the phenolic compounds in a liquid-liquid extraction. Thus, successive extraction with diethyl ether and then ethyl acetate has been used for phenolics in fruit juices (41). When using alcohol-water mixtures (40), repeated extraction or reflux for 1 h are necessary to extract free phenolic acids as well as their glycosides. 

Cyclonite is a white crystalline solid, m.p. 202°. It is insoluble in water, alcohol, ether, ethyl acetate, petroleum ether, and carbon tetrachloride, very slightly soluble in hot benzene, and soluble 1 part in about 135 parts of boiling xylene. It is readily soluble in hot aniline, phenol, ethyl benzoate, and nitrobenzene, from all of which it crystallizes in needles. It is moderately soluble in hot acetone, about 1 part in 8, and is conveniently recrystallized from this solvent from which it is deposited in beautiful, transparent, sparkling prisms. It dissolves very slowly in cold concentrated sulfuric acid, and the solution decomposes on standing. It dissolves readily in warm nitric acid (1.42 or stronger) and separates only partially again when the liquid is cooled. The chemical reactions of cyclonite indicate that the cyclotrimethylenetri-nitramine formula which Herz suggested for it is probably correct. 

Tannic and Gallic Acids.—A preliminary test for these two adds may be made by diluting the ink with water, acidifying slightly with dilute sulphuric add and extracting with ethyl acetate. The ethereal liquid is evaporated and the residue dissolved in water, the solution being tested as follows ... 

The methyl ethyl acetic acid may also be obtained by extraction of the acidified solution with ether. This method is not recommended, as small amounts of alcohol which are invariably present in this solvent, contaminate the product by the formation of the ethyl ester. 

TLC separation of DNS-amines is usually made on layers of silica gel with solvents covering a range of polarity, e.g., chloroform, ethyl acetate, diisopropyl ether and methanol. Seiler and Wiechmann [97] developed 30 solvent systems for the separation of DNS derivatives of over 100 biogenic amines on TLC plates of silica gel. The selective reaction of DNS-C1 with the amino group of catecholamines has been examined [98]. The drugs dopamine, norepinephrine and epinephrine are adsorbed on alumina which protects their hydroxyl groups from dansylation. The N-dansylated compounds are separated with benzene-dioxane-acetic acid (90 25 4) on layers of silica gel. 

Note Highly polar solvent sweet, ethereal odor soluble in water flammable, burns with a luminous flame highly toxic by ingestion, inhalation and skin absorption miscible with water, methanol, methyl acetate, ethyl acetate, acetone, ethers, acetamide solutions, chloroform, carbon tetrachloride, ethylene chloride, and many unsaturated hydrocarbons immiscible with many saturated hydrocarbons (petroleum fractions) dissolves some inorganic salts such as silver nitrate, lithium nitrate, magnesium bromide incompatible with strong oxidants hydrolyzes in the presence of aqueous bases and strong aqueous acids. Synonyms methyl cyanide, acetic acid nitrile, cyanomethane, ethylnitrile. 

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