Acetone water removal

Blending of samples with acetone and extraction with dichloromethane and acetone, water removal and volume reduction. Cleanup using carbon-celite (pasta) or C18 SPE (eggs). 

Finally, in the last step, the chelating auxiliary had to be removed Ideally, one would like to convert 4.54 into ketone 4.55 via a retro Mannich reaction. Unfortunately, repeated attempts to accomplish this failed. These attempts included refluxing in aqueous ethanol under acidic and basic conditions and refluxing in a 1 1 acetone - water mixture in the presence of excess paraformaldehyde under acidic conditions, in order to trap any liberated diamine. Tliese procedures were repeated under neutral conditions in the presence of copper(II)nitrate, but without success. 

Ma.nufa.cture. Mesityl oxide is produced by the Hquid-phase dehydration of diacetone alcohol ia the presence of acidic catalysts at 100—120°C and atmospheric pressure. As a precursor to MIBK, mesityl oxide is prepared ia this manner ia a distillation column ia which acetone is removed overhead and water-saturated mesityl oxide is produced from a side-draw. Suitable catalysts are phosphoric acid (177,178) and sulfuric acid (179,180). The kinetics of the reaction over phosphoric acid have been reported (181). 

Fig. 41. The pervaporation separation of acetone—water mixtures achieved with a water-selective poly(vinyl alcohol) (PVA) membrane and with an acetone-selective siUcone mbber membrane. The PVA membrane is best suited to removing small amounts of water from a concentrated acetone solution, whereas the siUcone mbber membrane is best suited to removing small amounts of acetone from a dilute acetone stream (89).

B-Norcholesterol Acetate (71). A test tube containing 2 g (4.4 mmoles) of (70) is placed in an oil bath at 150° and the temperature of the bath is slowly raised. At 170°, the liquified mass begins to froth and after 15 min the evolution of CO2 is essentially complete. The melt is allowed to stand at 180° for an additional 15 min. After cooling to room temperature and trituration with 5 ml of acetone, long white plates separate. The crystals are removed by filtration and washed with 70% acetone-water to yield 1.74 g (94%) of (71) mp 77-79°. 

The acetone was removed by evaporation in vacuo, and about 750 ml of water were added to dissolve the resulting residue. The solution was filtered. The potassium salt of N-p-ace-tylphenylsuifonyl-N -cyclohexylurea formed in the above reaction, being water-soluble, passed into the filtrate. Acidification of the filtrate with 6 N aqueous hydrochloric acid caused the precipitation of N-p-acetylphenylsulfonyl-N -cyclohexylurea which was collected by filtration. Recrystallization of the filter cake from 90% aqueous ethanol yielded purified N-p-acetylphenylsulfonyl-N -cyclohexylurea melting at about 188°-190°C. 

When addition is complete the mixture is heated under reflux during 5 hours and then the acetone is removed by distillation. The residue is dissolved in water, acidified with hydrochloric acid and the mixture extracted with chloroform. The chloroform extract is stirred with sodium hydrogen carbonate solution and the aqueous layer is separated. The alkaline extract is acidified with hydrochloric acid and filtered. The solid product is drained free from oil on a filter pump, then washed with petroleum ether (BP 40° to 60°C), and dried at 50°C. The solid residue, MP 114° to 116°C, may be crystallized from methanol (with the addition of charcoal) to give p-chlorophenoxyisobutyric acid, MP 118° to 119°C. 

The enamine protecting group was removed by dissolving 10 grams in aqueous acetone (250 ml water to 250 ml acetone) and vigorously stirring this solution at pH 2.5 for 1 hour. The acetone was removed in vacuo and the ester, which was salted out of the aqueous phase as a sticky yellow gum, was dissolved in ethyl acetate (200 ml) and washed twice with 200 ml portions of 1 N sodium bicarbonate and brine and dried over anhydrous magnesium sulfate. Careful addition of dry ester (about 50 ml) to the dry ethyl acetate layer... 

A solution of 25.8 g. (0.20 mole) of 4-amino-2,2,4-trimethyl-pentane (ierf-octylamine) (Note 1) in 500 ml. of C.P. acetone is placed in a 1-1. three-necked flask equipped with a Tru-Bore stirrer and a thermometer and is diluted with a solution of 30 g. of magnesium sulfate (Note 2) in 125 ml. of water. Potassium permanganate (190 g., 1.20 moles) is added to the well-stirred reaction mixture in small portions over a period of about 30 minutes (Note 3). During the addition the temperature of the mixture is maintained at 25-30° (Note 4), and the mixture is stirred for an additional 48 hours at this same temperature (Note 5). The reaction mixture is stirred under water-aspirator vacuum at an internal temperature of about 30° until most of the acetone is removed (Note 6). The resulting viscous mixture is steam-distilled approximately 500 ml. of water and a pale-blue organic layer are collected. The distillate is extracted with pentane, the extract is dried over anhydrous sodium sulfate, and the pentane is removed by distillation at atmospheric pressure. The residue is distilled through a column (Note 7) at reduced pressure to give 22-26 g. (69-82%) of colorless 4-nitro-2,2,4-trimethylpentane, b.p. 53-5473 mm., < 1.4314, m.p. 23.5-23.7°. 

Non-fatty foods (<2% fat, > 75% water) Extraction with acetone and removal of water with Flydromatrix oleanup using Florisil GC/ECD No data >85% ( r T sulfate) FDA 1994 (PAM Method 302)... 

Typically lipids, chlorophyll, and phenolic acids can be separated by liquid-liquid partition. Lipids and chlorophyll can be removed from acetone-water extracts by chloroform while phenolic acids have higher affinities for ethyl acetate at a pH close to nentral and water. °°... 

A 10-g sample of the homogenized dry sample is soaked in 20 mL of distilled water for 2 h. After adding 100 mL of acetone to the soaked sample and shaking vigorously on a mechanical shaker for 30 min, the extract is filtered. After the addition of a further 100 mL of acetone, the sample homogenate is shaken as before and the acetone extract is filtered. The filtrates are combined and acetone is removed with a rotary evaporator. " ... 

For cottonseeds, pyrithiobac-sodium is extracted with acetone-water (4 1, v/v). After filtration, the acetone is removed by evaporation under reduced pressure. The residue is adjusted to pH 1 and extracted with ethyl acetate. The extract is cleaned up by liquid-liquid partitioning and methylated with diazomethane. The methyl ester of pyrithiobac is purified by silica gel column chromatography. Pyrithiobac-methyl is determined by gas chromatography (GC) with nitrogen-phosphorus detection (NPD). 

The diamine was dissolved in N,N-dimethyl-acetamide by stirring under a nitrogen stream. After the diamine was completely dissolved, equal moles of isophthaloyl chloride was added all at once. Stirring was continued for about three hours after which the reaction mixture was poured into hot water and magnetically stirred. The polymer was washed with hot water at least three times and then extracted with acetone to remove low molecular weight species. The polymer was dried in vacuum oven at about 70°C overnight. 

Vinvlbenzvl Iodide—Vinylbenzyl chloride (20 g 0.131 mol) was added dropwise to dry sodium iodide (29.5 g 0.198 mol) in 130 mL dry acetone. The mixture was stirred at 50°C for 40 min, cooled to room temperature, and filtered. The acetone was removed by rotary evaporation, and 100 mL water and 150 mL ether were added to the solid residue. The aqueous layer was washed with ether. The combined ether layers were washed with water containing 2% sodium thiosulfate and dried over magnesium sulfate. The ether was removed by rotary evaporation and the yellow residue was dissolved in 50 mL hexane and cooled to -20°C. Within 1.5 hr, yellow crystals formed. Fast filtering with chilled glassware provided 17.1 g (53.5% of theory) of vinylbenzyl iodide. 

Prepare one 100-mL volumetric flask and five 25-mL volumetric flasks. These flasks should be clean and dry. They may be prepared by washing with soapy water and a brush, rinsing with water, removing the water with several rinses with acetone, and removing the acetone with several rinses with the alkane solvent to be used (e.g., hexane, heptane, or cyclohexane). 

Abstract In this study, a new natural adsorbent (sumae leaves) for removing Cu (II) ion from the aqueous solutions has been investigated. Leaves of sumae were obtained from Siirt, Tmkey. The tannins were extraeted with acetone water (70 30, v/v) mixture from the leaves of sumac. For the total tannin determination Folin-Ciocalteu method was used and tannin content was found 27%. In batch experiments, pH profile, adsorption time, adsorbent/hquid ratio, initial concentration of metal ions, adsorbent amoimt, particle size of adsorbent and temperature were performed to determine binding properties of adsorbent for the Cu(II) ions. The concentrations of the metal ions in solutions before and after adsorption were measured with an atomic absorption spectrophotometer. 

Leaves of Sumac were used for removal of ions in aqueous solution. Tannins were extracted from the leaves of sumac by extracting with 70% (v/v) acetone-water solution. For the total tarmin determination Folin-Ciocalteu method was used and tannin content was found 27%. Various adsorption parameters for the effective removal of Cu + ions by using sumac leaves as an adsorbent from aqueous solutions were studied and optimized. 

The other change that needed to be made in the synthesis of RSR 13 for in vivo administration was the method of purification. RSR 13 is used in vivo as the sodium salt. I prepared the first batch for in vivo toxicology by triturating RSR 13 sodium salt with acetone to remove any vestiges of water. However, the first industrial scale-up procedure called for crystallization of the salt from ethanol-water. The ethanol-water crystals were not as soluble as the acetone triturated method and could not be formulated at a reasonable volume. We performed the crystal structure determination of the ethanol-water crystals and found that it was a heptahydrate (Figure 17.5) [50]. The problem for large-scale production of RS R13 was solved eventually by the industrial producers of RSR 13. 

We have employed two different protocols for the chemical fractionation of GSE obtained from MegaNatural-AZ based on the amounts needed for bioactivity-based assays. Batches of GSE (50 g) were extracted in acetone/water (7 3) under N2 with mechanical agitation for 12 h. The acetone was removed on a rotary evaporator and the aqueous phase was freeze-dried to yield 48 g of tannin crude extract (TCE). TCE was further fractionated following two different methods. 

After 15 hr the acetone is removed on a rotary evaporator and water (125... 

B. 7-Fluoroisatin (3). A 250-mL, three-necked, round-bottomed flask fitted with a condenser and a thermometer is charged with 100 mL of coned sulfuric acid. After heating to 70°C, 30.0 g (0.165 mol) of anilide 2 (Note 9) is added over a period of 1 hr. The resulting deep red solution is heated to 90°C (Note 10) for 60 min (Note 11) and then is cooled to room temperature (20°C) over an ice bath (Note 12). The mixture is then added rapidly to a vigorously stirred mixture of 1.0 L of ice water and 200 mL of ethyl acetate (Note 13). The organic phase is separated and the almost black aqueous phase is extracted twice with 200 mL of ethyl acetate (Note 14). The combined red organic phases are dried with sodium sulfate. The solvent is removed under reduced pressure and the crude product is dried at low pressure, whereupon 12.9 to 15.7 g (47-57%) of an orange powder, mp 186-190°C, is obtained (Note 15). The crude product is sufficiently pure for the next step. Further purification is possible by recrystallization from acetone/water. 

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