Extraction, viii

Magnusson, G., S. Thoren, J. Dahmen, and K. Leander Fungal Extractives. VIII. Two Sesquiterpene Furans from Lactarius. Acta Chem. Scand., B 28, 841 (1974). 

A mixture of 0.10 mol of freshly distilled 3-methyl-3-chloro-l-butyne (see Chapter VIII-3, Exp. 5) and 170 ml of dry diethyl ether was cooled to -100°C and 0.10 mol of butyllithium in about 70 ml of hexane was added at this temperature in 10 min. Five minutes later 0.10 mol of dimethyl disulfide was introduced within 1 min with cooling betv/een -100 and -90°C. The cooling bath vjas subsequently removed and the temperature was allowed to rise. Above -25°C the clear light--brown solution became turbid and later a white precipitate was formed. When the temperature had reached lO C, the reaction mixture was hydrolyzed by addition of 200 ml of water. The organic layer and one ethereal extract were dried over potassium carbonate and subsequently concentrated in a water-pump vacuum (bath... 

A mixture of 0.25 mol of l,4-diethoxy-2-butyne (see Chapter VIII-6, Exp. 8) and 100 ml of dry diethyl ether was cooled at -45°C. A solution of 0.55 mol (note 1) of ethyllithium (note 2) (see Chapter II, Exp. 1) in about 450 ml of diethyl ether was added in 30 min. The temperature of the mixture was kept between -45 and -35°C. After the addition the mixture was stirred for an additional 20 min at -40°C. The light brown solution was then poured into 500 ml of ice-water, which had been saturated with nitrogen (note 3). After shaking the upper layer was separated off and the agueous layer was extracted twice with small portions of diethyl ether. 

To a suspension of a tinc-copper couple in 150 ml of 100 ethanol, prepared from 80 g of zinc powder (see Chapter II, Exp. 18), was added at room temperature 0.10 mol of the acetylenic chloride (see Chapter VIII-2, Exp. 7). After a few minutes an exothermic reaction started and the temperature rose to 45-50°C (note 1). When this reaction had subsided, the mixture was cooled to 35-40°C and 0,40 mol of the chloride was added over a period of 15 min, while maintaining the temperature around 40°C (occasional cooling). After the addition stirring was continued for 30 min at 55°C, then the mixture was cooled to room temperature and the upper layer was decanted off. The black slurry of zinc was rinsed five times with 50-ml portions of diethyl ether. The alcoholic solution and the extracts were combined and washed three times with 100-ml portions of 2 N HCl, saturated with ammonium chloride. 

A suspension of sodium amide in 500 ml of anhydrous liquid artmonia was prepared from 18 g of sodium (see Chapter II, Exp. 11). To the suspension was added in 10 min with swirling a mixture of 0.30 mol of 1-chloro-l-ethynylcyclohexane (see VIII-2, Exp. 27) and 50 ml of diethyl ether. The reaction was very vigorous and a thick suspension was formed. The greater part of the ammonia was evaporated by placing the flask in a water bath at 50°C. After addition of 500 ml of ice-water the product was extracted three times with diethyl ether. The ethereal extracts were dried over anhydrous KjCOj and subsequently concentrated in a water-pum vacuum. Distillation of the residue afforded the amine, b.p. 54°C/15 mmHg, n 1.4345, in 87% yield. 

The HMR/fractionatlon approach gives very good results When applied to ethylene-propylene copolymer fractions reported by Abls, et. al. (19) These authors extracted sample 5 (In Table VII) with hexane to get soluble and Insoluble fractions (5a and 5b), and with ether to get soluble and insoluble fractions (5c and 5d). The hexane set (5a and 5b) and the ether set (5c and 5d) can be separately analyzed by the HIXCO.TRIADX program. The results are shown In Table VIII. In the 2-state (B/B) model, we have 4 parameters and 12 values to fit to HMR data of pairwise fractions. In the 3-state (B/B/B) model, we have 7 parameters and 12 values to fit. Thus, the use of pairwise fractions Is absolutely essential for 3-state analysis. 

M. Current evidence Indicates that the effect may be ascribed to the formation of a TIO film on the surface of the group VIII metal particles (6,7) Whatever the cause of the SMSI state. It Is certainly the case that It has altered site energetics and possibly their density on the catalysts. The extraction of site... 

Lemna obscura fronds contain high quantities of anthocyanln that are extractable by soaking the fronds In 0.1 M HC1. L. obscura growth in the culture dish bloassay was similar to that of L. minor and appeared to be more sensitive to low levels of allelochemlcals. Anthocyanln concentration was affected by low concentrations of salicylic acid (Table VIII). Final frond number and dry weight were consistently reduced by 100 pM and 500 pM concentrations of salicylic acid whereas anthocyanln formation was inhibited by 50 UM concentrations of salicylic acid and stimulated by 0.5 VM. 

Table VIII. The effect of three fractions separated from extracts of tall fescue (pH 5.5) ...

Table VIII. Effect of Ragweed Organic Solvent Extracts on Lettuce and Carrot Germination...

The structures under consideration are indicated in Inserts VI and VII. Such radicals are usually secondary products of radiolysis, formed, for example, by extraction of hydrogen from a R2C(H)-precursor. However, closely related radicals can be formed, for example, by electron-loss from vinyl- or allyl- derivatives (66,67) or from substituted aromatic cations (68,69) [see, for example, VIII-X]. 

Almela, A. Elizalde, M. P. Interactions of metal extractant reagents. Part VIII. Comparative aggregation equilibria of Cyanex 302 and Cyanex 301 in heptane. Anal. Proc. 1995, 32, 145-147. 

DMA in 500 ml ether mix rapidly with 270 ml 0.9 M phenyl-Li, boil fifteen hours and extract as for (VI) or as described previously to get 8 g oily 4-methoxy-indoline (or its 1-methyl derivative) (VII). Alternatively, add 36 g naphthalene to 300 ml tetrahydrofuran and add 11 g Na metal cut in small pieces. Reflux and stir three hours and add 18 g (VI) and 8 g DEA in 200 ml tetrahydrofuran rapidly and boil twelve hours. Evaporate in vacuum, dissolve the oily residue in 2N HCI and extract with ether. Proceed as described to get (VII). 4 g (VII) in 200 ml dry pyridine add to 6 g Cu chloride in 400 ml pyridine and reflux 1 xh hours. Pour on water and extract with ether. Wash extract with 4N HCI and then water and dry and evaporate in vacuum the ether to get 2 g of the indole (VIII). Alternatively, dissolve 4 g (VII) and 9.5 g cinnamic acid in 700 ml mesitylene, add 1 g 5% palladium-carbon and reflux five hours. Filter, wash with HCI and NaHC03 and dry and evaporate in vacuum the mesitylene to get the red, oily (VIII) (can chromatograph on alumina and elute with benzene-petroleum ether). 

All MS technologies require the establishment of method-specific mass libraries so that compounds in the spectra can be identified [212], a tedious task that has been restricted to large laboratories. Nevertheless, some of these efforts are driven by the metabolomics community, thereby requiring some sort of standardization to conduct comparable experiments, as has been proposed with the ArMet standard [216], Last but not the least, metabolomics experiments generate large amounts of data that need sophisticated analysis methods to extract biological information, usually based on multidimensional statistics [3, 5, 58, 209, 217, 218]. Metabolomics experiments as the basis for an analysis of the possible dynamics of metabolic networks are discussed in Section VIII. 

When compound (VII) was heated to 130° for 2-5 hr. it isomerized to OO -diethyl S-ethylmercaptoethyl phosphoro-thiolate (VIII). This was shown by successive partitioning of the heated product between suitable solvents, the partition ratios of the radioactive phosphorus being determined after each extraction. If only one compound is present all the ratios would be the same if two or more compounds are present, the observed over-all partition ratios would change in systematic fashion. 

The Mississippi cotton was much more difficult to wet out than either the California or Texas cottons. This is apparently related to the nature of noncelluloslc constituents on the fiber surfaces. The Mississippi cotton was a mature, low noncellulose content cotton, whereas, both the California and Texas cottons had high noncellulose contents. The ratio of wax content to total noncellulosics was much higher for the Mississippi cotton than for either the California or Texas cottons. The surface of the Mississippi cotton is thus more hydrophobic and resists wetting, Levels of extractables and dust levels are summarized in Table VIII. 

Osmium(viii).—From studies of the extraction of OSO4 from alkaline aqueous solutions by carbon tetrachloride, it has been suggested that the anion [0s04(0H)] may exist in these media. Similar evidence was found for the presence of [OsOjN]" in aqueous ammonia solutions of 0s04. Examination of the i.r. spectra of a series of metal complexes of the ligand 8-amino-7-hydroxy-4-methylcoumarin, including [OsO LjjClj, indicate a correlation between certain vibrational bands, e.g. v(M—N), and the stability of the compounds. ... 

Phenylpropanamide (130), from the aposematic beetle (genus Metrior-rhynchus) (Table VIII), has been purified by gas chromatography from the methanol extract. Its structure is presumed from mass spectral data and was confirmed by comparison with a synthetic sample (97). The co-occurrence of amide 130 and l-methyl-2-quinolone (57) in this beetle suggests a common pathway of biosynthesis and that they may be derived from the amino acid phenylalanine. 

Therapy is determined by the level of factor VIII deficiency. Severely affected patients have concentrations less than 1 %, in moderate disease this is present between 1 and 5 % whereas plasma levels between 5 and 30 % may be associated with bleeding only after trauma such as dental extraction. Additionally, the choice of replacement is modified by the site of bleeding and the presence or absence of inhibitors that interfere with the function of the factor. Cryoprecipitate or lyophilised concentrate is becom-... 

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