Carbon extraction

To a mixture of 10 g. of the compound and 3-5 ml. of 33 per cent, sodium hydroxide solution in a test-tube, add 2-5 ml. of 50 per cent, chloroacetic acid solution. If necessary, add a little water to dissolve the sodium salt of the phenol. Stopper the test-tube loosely and heat on agently-boiling water bath for an hour. After cooling, dilute with 10 ml. of water, acidify to Congo red with dilute hydrochloric acid, and extract with 30 ml. of ether. Wash the ethereal extract with 10 ml, of water, and extract the aryloxyacetic acid b shaking with 25 ml. of 5 per cent, sodium carbonate solution. Acidify the sodium carbonate extract (to Congo red) with dilute hydrochloric acid, collect the aryloxyacetic acid which separates, and recrystallise it from hot water. 

A suspension of 17a,21-dihydroxypregna-4,9(ll)-diene-3,20-dione 21-acetate (0.77 g) and iV-bromoacetamide (0.3 g) in anhydrous methylene dichloride (40 ml) is added over 2-3 min with stirring to a mixture of anhydrous hydrogen fluoride (10.19 g), and anhydrous tetrahydrofuran (18 g) in a polyethylene bottle at —80° (acetone-dry ice). After 1 hr at —80° the reaction mixture is kept for a further 1 hr at 0° and then added cautiously to an excess of an ice-cold solution of sodium carbonate. Extraction with methylene dichloride and crystallization from acetone-hexane furnish 9a-bromo-ll -fluoro-17a,21-dihydroxypregn-4-ene-3,20-dione 21-acetate (0.69 g), mp 205-208°, raised by several crystallizations from acetone-hexane to 215-217° [aju 142° (CHCI3) max 240-242 mju (e 15,500). 

Step 1 1-(p-Chlorophenyl)-3-Ethoxy-1 H-lsoindole - Crystalline triethyloxonium boron-tetrafluoride (21 g) (prepared from 23 g of borontrifluoride etherate and 11 g of epichlorohydrin) is dissolved in 100 ml of absolute methylenechloride. 3-(p-Chlorophenyl) phthalimidine (21 g) is added and the reaction mixture is stirred overnight at room temperature. The resulting solution is poured onto 50 ml of saturated Sodium carbonate, extracted with 500 ml of ether and dried. Upon evaporation of the solvent there is obtained crude material which is recrystallized from methylene chloride/hexane (1 1) to yield l-(p-chlorophenyl)-3-ethoxy-1 H-isoindole MP 102° to 103°C. 

An additional 5-8 g. of slightly colored material can be secured by neutralizing the aqueous solution with 200 g. of sodium carbonate, extracting with 500 ml. of ether, and distilling. The total yield of distilled product then amounts to 125-130 g. (95-97%). 

In many SSD procedures, one of the important steps, which is still problematic, is carbonate -extraction. This chemical component is an abundant constituent of soils, particularly in the arid regions. It contains a... 

Dissolve 27 g 4,5, or 6 methoxy (or ethoxy, methyl, etc.) tryptophan in 50 ml freshly distilled acetaldehyde and 1 L water and heat at 50° in loosely stoppered flask three hours. Heat on steam bath five hours to remove acetaldehyde, then add 5 L water and heat to boiling. Add 1.2 L 10% K dichromate and 240 ml glacial acetic acid and continue heating three minutes. Cool and add excess Na sulfite take pH to 8 with Na carbonate Extract with 5 L ether and dry, evaporate in vacuum (or simply evaporate in vacuum after cooling) to get the harmaline isomer. 

TABLE 3-1 Extraction Efficiencies (ef) and Organic Carbon Extraction Efficiencies (ocef) of Various Solvents and Binary Mixtures for Atmospheric Aerosol Samples"... 

Ground calcium carbonate, extracted from the earth, is present in practically every country in the world in varying quantities in the form of limestone, marble, dolomite or chalk. Following the extraction, GCC needs to be ground. Dry grinding, the cheaper alternative, is often limited to a minimum particle size of 2- 3 microns. Wet grinding, more expensive, is used for fine and ultra fine material or when the final product must be a slurry (paper or paint application). Precipitated calcium carbonate is produced by chemical reaction between... 

The filtrate, ca. 4 1. in volume, is extracted with three 1.5-1. portions of ether (Note 4), and the sulfuric acid mother liquors are discarded. The ether extracts are combined and used to dissolve the solid mixture of acid and ester. If necessary, more ether can be added to assist in dissolving the solid. The ether solution is washed with 50 ml. of cold water and extracted with approximately ten 100-ml. portions of saturated sodium carbonate solution until all the isodehydroacetic acid has been removed (Note 5). The combined sodium carbonate extracts are acidified with an excess of concentrated hydrochloric acid, and the finely divided acid which precipitates is redissolved by heating to the boiling point. The hot solution is filtered with the aid of suction and is cooled in an ice bath the solid is collected on a filter. The crude isodehydroacetic acid is dissolved in 400 ml. of hot water, and this solution treated with decolorizing carbon, filtered, and cooled slowly to effect crystallization. The yield of isodehydroacetic acid is 91-115 g. (22-27%) m.p. 154-155°. 

The unacceptable taste and odor of drinking water from a tributary of the upper Ohio River led Frank Middleton and his collaborators in the U.S. Public Health Service to apply their granular carbon extraction-chloroform elution procedure to obtain residue samples of that water in 1962 (2). The first preliminary suggestions that such residues were carcinogenic were presented by Hueper and Payne (3) the following year. For whatever reason, those observations appeared to have had little impact. 

Suppose an archeologist extracts 1.0 g of carbon from an ancient ax handle and finds that carbon to be one-fourth as radioactive as 1.0 g of carbon extracted from a freshly cut tree branch. About how old is the ax handle ... 

Phenyl -tolyl selenide in aqueous suspension is boiled with potassium permanganate for several hours. The manganese mud is dissolved and the 4-carboxydiphenyl selenoxide precipitated by passing in sulphur dioxide. After filtration the precipitate is macerated with dilute sodium carbonate solution, the products of oxidation being separated in this manner into phenyl p-tolyl selenoxide and 4-carboxydiphenyl selenoxide. Addition of dilute sulphuric acid to the sodium carbonate extract causes the separation of 4-carboxydiphenyl selenoxide, which is crystallised from alcohol. The product is a microcrystalline powder, melting with decomposition at 253° to 255° C. Attempts to resolve it into optically active forms have failed the l-menthylamine salt melts at 220° to 222° C. with decomposition, and the d-a-phenyl-ethylamine salt forms feathery needles, M.pt. 194° to 195° C. with decomposition.3... 

Methylnitramine is conveniently prepared3 by nitrating methylurethane with absolute nitric acid, drowning in water, neutralizing with sodium carbonate, extracting with ether, and... 

The sodium carbonate extract contains only a few milligrams of the enedione. 

The oxidation procedure described affords a mixture of acids from which no component is easily isolable. When the oxidation is allowed to proceed in the temperature range 18-5° for 15-22 hours, as described in Note 1, isolation of the Diels acid (3,4-seco-A5-cholesten-3,4-dioic acid) is easily accomplished as follows. The carbonate extract is acidified and shaken with ether, and the clear aqueous layer is discarded. The ethereal solution, which may contain some suspended Diels acid, is not dried but is run into a flask and diluted with an equal volume of acetone. The mixture is evaporated to a volume of 15-20 ml. and cooled, and the Diels acid is collected as a white powder, m.p. 280-285° yield 0.5 g. 

Calcium carbonate Extraction of iron, making cement, glass making... 

Reduction with zinc powder and acid. Simple p-quinones are reduced to hydro-quinones in the following manner. Dissolve or suspend 0.5 g of the quinone in dilute hydrochloric acid (1 5) and add a little zinc powder. When the solution is colourless, filter, neutralise with sodium hydrogen carbonate, extract the dihyd-ric phenol with ether, remove the solvent and identify (Section 9.6.6, p. 1248). 

Cool the alkaline solution resulting from the distillation of the volatile neutral compounds, make it acid to litmus with dilute sulphuric acid and add an excess of solid sodium hydrogen carbonate. Extract this hydrogen carbonate solution with two 20 ml portions of ether remove the ether from the combined ether extracts and identify the residual phenol (or enol). Then acidify the hydrogen carbonate solution cautiously with dilute sulphuric acid if an acidic compound separates, remove it by two extractions with 20 ml portions of ether if the... 

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