Acetyl, acetone extractions

Aluminium Extraction with trifluoro-acetyl acetone in toluene Analysis of toluene extract by GC 6 pg A1 in 2 xl extract [18]... 

The acetonation was carried out on the entire distillate, thereby avoiding the steps of decolorization, concentration and acetone extraction. The acetonated mixture was extracted directly with chloroform, care being taken to minimize the possibility of hydrolysis of the 3,4-isopropyl-idene-D-galactosan<1,5>/3<1,6> while in the presence of the residual sirups. Acetylation of the chloroform-insoluble residue, followed by vacuum distillation, yielded crystalline triacetyl D-galactosan <1,4 >a-... 

When the distribution equilibrium reaction involves hydrogen ions, changing the hydrogen ion concentration will have a strong effect on the distribution coefficient. An example of this is the extraction of metal complexes of acetyl acetone (HAa) and other weakly acid complexing agents by benzene. The equilibrium reaction for extraction of thorium by this reagent is... 

The solvent extraction study was performed between pH 1 and 11, using acetyl acetonate as complexing extractant and toluene as organic phase. The solvent extraction data cannot be evaluated quantitatively since insufficient experiment detail was reported. 

Extractant 283 CgHg02 Acetyl acetone (1,4-pentadione), HA Distribution constants ... 

VAc. See Vinyl acetate VACAC. See Vanadium tris acetyl acetonate Vaccinium myrtillus Vaccinium myrtillus extract. See Bilberry (Vaccinium myrtillus) extract... 

The solvent system is ethyl acetate ethanol water=3 l 3, with heavy phase as the stationary phase, the light phase as mobile phase the solute acetyl acetone (AR) acetyl acetone solution 5 mg/ml as the feed liquid automatic fraction collector spiral countercurrent extraction device ... 

The importance of the solvent as an environmental factor was inferred by extraction experiments. A solution of /-[Co(acac)3] (acac = acetyl-acetone) in CCl3H-EtOEt mixture was extracted with 2% d-[Co(en)3]l3 saturated with ether. The portions extracted into the aqueous layer were then extracted quantitatively with CHCI3 and evaporated. The green residue... 

The interferences of aluminum, sodium fluoride, and iron(lll) have been studied [13]. The results indicate that lowering the pH is recommended. Only small amounts of Fe(lll) can be present as higher concentrations could be removed by extraction with acetyl acetone complex with CCU-... 

A solution of 1.05 M diborane in THF (25 ml, 26 mraol) was added slowly to a stirred suspension of 3-acetyl-5-hydroxy-2-methylindole (1.0 g, 5.3 mmol) in THF (10 ml). After hydrogen evolution ceased, the mixture was heated at reflux for I h, cooled and poured into acetone (75 ml). The mixture was heated briefly to boiling and then evaporated in vacuo. The residue was heated with methanol (50ml) for 20min. The solution was concentrated and 3NHC1 (40ml) was added. The mixture was extracted with ether and the extracts dried (MgSO ) and evaporated to yield a yellow oil. Vacuum sublimation or recrystallization yielded pure product (0.76 g, 82%). 

Preparation of 9, 11 -Epoxy-17a-21 -Dihydroxy-16 -Methyl-4-Pregnene-3 0-Dione 21-Acetate To a stirred solution of 100 mg of the 9a-bromo-11(3,17a,2Ttrihydroxy-16 3-methyl-4-pregnene-3,20-dione 21-acetate in 3 ml of tetrahydrofuran and 1 ml of methanol under nitrogen was added 1.02 ml of 0.215 N methanolic sodium methoxide. After 10 minutes at 25°C, 0.2 ml of acetic acid was added and the methanol removed in vacuo. The residue was acetylated with 1.00 ml of pyridine and 0.5 ml of acetic anhydride at 60°C for 70 minutes. The mixture was taken to dryness in vacuo, water added, and the product extracted into chloroform. The residue was crystallized from ether-acetone to give pure 9(3,11 (3-epoxy-17a,21-dihydroxy-16(3-methyl-4-pregnene-3,20-dione 21-acetate. 

The solubility of iridoids depends on their state (free, glycosylated, acetylated), but usually they are extracted with polar solvents methanol, ethanol, aqueous alcohols, and rarely acetone. Iridoid glycosides are more or less stable some of them are very sensitive to acids and alkalis. Some iridoid glycosides such as aucubin suffer color modification after chemical or enzymatic hydrolysis they give first a blue to green... 

Convert indole to indolyl-3-methyl-ketone (I) by treating indolyl-Mg-Br (preparation already described) with acetyl-Cl, by treating indole in POCl3 with dimethylacetamide (Vilsmeier reaction), or by reacting indole with diketene (ACS 22,1064(1968)). 15.9 g (1) in 50 ml methanol cool, stir and add dropwise 16 g Br2. Reflux 1 Vi hours on water bath cool, filter, wash with ether and recrystallize-methanol to get 18 g indolyl-3-Br-methyl-ketone (II). Dissolve 11.9 g (II) in 60 ml warm isopropanol and add 11 g 3 8% aqueous DMA (or equimoiar amount other amine) reflux one hour on water bath. Filter (recrystallize-ethanol) to get 8.5 g indolyl-3-dimethylamino-methyl ketone (III). Add 4.6 g (0.02 M) (III) in 30 ml tetrahydrofuran to 2.3 g lithium aluminum hydride in 50 ml tetrahydrofuran, stir one-half hour at room temperature and reflux two hours. Add a little water dropwise and extract the precipitate with acetone. Dry, evaporate in vacuum the combined organic phases to get an oil which will precipitate with ether-petroleum ether to give DMT. (Ill) should be tested for psychedelic activity. Dialkyltryptamines BCSJ 11,221 (1936), BSC 2291 (1966)... 

A (Alternative) JCS 3175(1952). 2 g 3-indolyl-acetic acid (preparation given elsewhere here), 1.55 g freshly fused sodium acetate, 5 ml acetic anhydride. Heat 135-140° on oil bath for eighteen hours cool, wash with water and extract with CHCl3-ether (1 4). Wash organic phase with 3X20 ml saturated KHC03 and dry, evaporate in vacuum to get the l-acetyl-3-indolyl-acetone, which can be reduced to the alpha-methyl-tryptophol derivative with lithium aluminum hydride, and then converted to the dialkyl-tryptamine as already described (as can (I)), or used in step B, or reduced to (I) as follows dissolve 1 g in 1 ml 1 N Na-methoxide in methanol and 60 ml methanol, and keep at 40° for 10 minutes acidify with dilute HC1 and extract with ether. Dry, evaporate in vacuum to get (I) (recrystallize-methanol). 

Lee [42] determined pentachlorophenol and 19 other chlorinated phenols in sediments. Acidified sediment samples were Soxhlet extracted (acetone-hexane), back extracted into potassium bicarbonate, acetylated with acetic anhydride and re-extracted into petroleum ether for gas chromatographic analysis using an electron capture or a mass spectrometric detector. Procedures were validated with spiked sediment samples at 100,10 and lng chlorophenols per g. Recoveries of monochlorophenols and polychlorophenols (including dichlorophenols) were 65-85% and 80-95%, respectively. However, chloromethyl phenols were less than 50% recovered and results for phenol itself were very variable. The estimated lower detection limit was about 0.2ng per g. 

The butanol-acetone fermentation, using whey supplemented with yeast extract, is substantially a butanol fermentation. Volatile solvents from the fermentation consist of 80% butanol, 13% acetone, and 5% ethanol. Approximately 30% of the lactose that is fermented is converted to butanol, 5% to acetone, 2% to ethanol, and the balance largely to CO2 and small quantities of butyric and acetic acids, acetyl-methylcarbinol, and hydrogen. 

To a stirred slurry of 63.47 g (0.177 mole) of 3 -[(2-imino-3-thiazolidinyl) acetyl]acetanilide hydrobromide in 1 L of 95% ethanol, maintained at 5°C, is added 5.70 g (0.15 mole) of sodium borohyride. After stirring 40 min an additional 4.10 g of sodium borohydride is added and the mixture is acidified with hydrochloric acid and evaporated under reduced pressure. The residue is partitioned between chloroform and dilute aqueous ammonium hydroxide. Two further chloroform extracts are combined with the original, washed with brine, dried (sodium sulfate) and evaporated to give an oil. Treatment with acetone gives 6.77 g (48%) of 3 -[l-hydroxy-2-(2-imino-3-... 

Mono, di and triethylene glycols Mixtures of water and dioxane or acetone Nitrile- Flame siloxane ionisation rubber Solvent extract acetylated in presence ofBF4 2mg L1 [224]... 

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