Diethyl ether earths

Copper powder. Hydrochloric acid. Methanol, Diethyl ether, Mesitylene, Trichlorotrinitrobenzene, Picrylchloride, Diatomaceous earth. Activated charcoal. Acetone... 

Rare earth acetylacetonates can be prepared from the metal oxide and acetylacetone however, the degree of hydration of the products depends on the experimental conditions. Trihydrates precipitate from 60% aqueous ethanol, dihydrates from cold 95% ethanol and monohydrates from hot 95% ethanol.180 An extensive series of hydrated lanthanide hexafluoroacetylacetonates has been prepared from the appropriate metal oxide and NH4 CF3COCHCOCFf, I8I 183 Trimeric [U02(CF3-COCHCOCF3)2]3 may be prepared from U03 2H20 and hexafluoroacetylacetone in diethyl ether. An etherate is initially isolated which protects the product from hydrolysis but which can be readily desolvated by heating in vacuum.184 Tested syntheses of the tris(tetramethylheptanedionates) of Sc, Y, La, Pr, Nd, Sm, Eu and Gd have been published.185... 

A cooled mixture of 20 ml of absolute methanol in 200 ml of methylene chloride is added within 30 minutes, after another 30 minutes the precipitate is filtered off under exclusion of moisture, washed with methylene chloride and dried under reduced pressure at room temperature. The obtained hygroscopic crystals of the hydrochloride of 7p-[D-a-(l,4-cyclohexadienyl)-acetylamino]-3-methoxy-3-cephem-4-carboxylic acid are stirred into 200 ml of ice water and the milky solution treated with about 66 ml of cold 2 N sodium hydroxide solution until pH 3.5 is reached. The solution is clarified by filtration through diatomaceous earth, washed with ice water, cooled to 0°C and treated with 20 ml of 2 N sodium hydroxide solution until pH 5.7 is reached. A second filtration through a glass filter frit results in a clear solution which is treated with acetone (800 ml) at 0°C. The crystals are filtered washed with acetone water (2 1), acetone and diethyl ether and dried for 20 hours at room temperature and 0.05 mm Hg to give the 7p-[D-a-amino-a-(l,4-cyclohexadienyl)-acetylamino]-3-methoxy-3-cephem-4-carboxylic acid dihydrate. 

The first of these, utilized by Yoder, McCalip and Seibert,34 and by Balch, Broeg and Ambler,37 provides for the extraction of the aconitic acid from the sample being investigated, usually with diethyl ether, and the subsequent isolation of the acid from the solvent. In dealing with solid samples, e.g. alkaline earth aconitates, evaporator scale, etc., the prescribed procedure is to dissolve the material in aqueous mineral acid and to extract the acid solution exhaustively with ether. The ether extract is then evaporated under reduced pressure, the dried residue titrated with standard alkali and the titratable acid calculated as aconitic acid. In dealing with such solid samples it is often necessary to make an additional determination for oxalic acid which otherwise would be assumed to be aconitic acid.37 The aconitic acid in liquid samples is usually precipitated as the insoluble lead salt which is separated and treated as any other solid sample. In some cases this procedure is unnecessary and the liquid samples are merely acidified with a mineral acid and then extracted with ether.37 This method for the determination of aconitic acid, however, requires a considerable amount of time and is further complicated by the interference of ether-soluble waxes and non-volatile acids. 

For reductions carried out in the absence of an added proton donor the usual solvents are liquid NH3, usually with an ethereal cosolvent, or less commonly an ether (THF, DME or diethyl ether). TTie reducing agent is usually one of the common alkali metals (Li, Na, K), although Rb, Cs and alkaline earth metals have also been used. " At least in the case of camphor both types of solvent systems give similar ratios of epimeric alcohols however, product ratios may vaiy as a function of the metal used as reducing agent. In reductions carried out in ethereal solvents the use of ultrasound increases the rate of the reaction, but does not affect the product distribution. ... 

Anhydrous samarium(III) chloride [Rare Earth Products, Johnson Matthey] (2.40 g, 9.40 mmol) is placed in a 200-mL Schlenk tube containing a magnetic stirring bar. Tetrahydrofuran (THF) (100 mL) is introduced via a cannula at 20 °C. The mixture is stirred at 20 °C for 2 h. Solid (2,6-di-tert-butylphenoxo)-lithium-diethyl etherate (8.13g, 28.4 mmol) is added to this slurry at 20 °C. A reflux condenser is then fitted to the Schlenk tube, and the reaction mixture is heated under reflux for 8 h. After h, the solid dissolves to yield a clear yellow-green solution. The solvent is removed at 25 °C and 10 torr, leaving a yellow-green solid, which is scraped from the sides of the Schlenk tube with a spatula and transferred to a sublimation tube. Sublimation at 255-260°C and 10 torr affords yellow crystals of tris(2,6-di-tert-butyl-phenoxo)samarium. Yield 4.46 g (62%). ... 

All Sc may be extracted with diethyl ether from an acidic solution (0.1-0.2 M HCl) containing 50% NH4SCN. Rare-earth elements remain in the aqueous solution [6]. 

An ammonium polysulfide solution is prepared as in Section 3-A above to this solution is added 3.00 g K2PdCl4 (9.18 mmole) dissolved in 10 mL water. After shaking for 2 minutes, the initial black precipitate redissolves, and the solution is filtered through diatomaceous earth (filter aid or Celite) prewashed with ammonium hydroxide. The filtrate is stoppered and the reaction allowed to proceed 5 days at room temperature (ca. 22°). At this time, the solution is noticeably lighter in color and the product has precipitated. After filtration, the complex is washed with water, ethanol, diethyl ether, carbon disulfide, and... 

Sample preparation Place 100 p-L 100 p,M diclofenac in dichloromethane in the bottom of a tube and evaporate it to dryness under a stream of nitrogen, add 100 p-L plasma, add 25 pL 1 M HCl, mix, add to a dry Chem Elut diatomaceous earth SPE cartridge (Varian), let stand for 5 min, elute with 6 mL n-hexane diethyl ether isopropanol 50 ... 

The reaction of resorcinol with prenyl halides in ethereal solution containing alkali metals or alkaline earth metals or their hydroxides has been instanced among a range of other compounds (ref. 11). By contrast the reagent, isoprene-magnesium-diethyl ether (ref.4) with either resorcinol (R = OH,R = H) or catechol (R = H, R = OH) only afforded chroman products. 

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