Isopropanol wash

A 2 cm length of isopropanol-washed copper wire was vapor-deposited onto 1 X 3 sections of silicon wafer at a pressure of about 10 5 Torr. The composition of the copper films was determined via XPS to be 99% cuprous oxide. The mirrors were then stored in a desiccator for up to 1 month without any change in composition. Next, a 0.01 M solution of stearyl thioglycolate in isopropanol was prepared. A single, isopropanol-rinsed copper mirror was then immersed into 200 ml of the stearyl thioglycolate solution for 10 min. The mirror was then removed from the solution, air-dried horizontally, and finally immersed into a swirling bath of pure isopropanol for about 30 s. After being air-dried, experimental analysis was then conducted on the prepared films. 

Wash kinetics of contaminated hair and hair from a drug user. Hair treatments , dry isopropanol washes , phosphate buffer , enzymatic digestion. 

It should be noted that in this definition all contribution from contamination present in the accessible domain (isopropanol wash) has been excluded. This is done to enhance the precision of the definition, i.e., to shield Rgsz from the possible influence of the widely varying drug concentrations in the accessible domain. These concentrations can range from zero in freshly shampooed hair to a very large number in freshly contaminated hair. The effective differentiation between drugs present in the accessible and semiaccessible domains is made possible by the dramatic difference in the cleansing power of dry isopropanol (as well as ethanol) and water. This distinction, however, cannot be achieved with methanol, since this resembles water in its wash properties. 

DNA template preparations are a major source of contamination in cell-free synthesis. In vitro translation reactions are sensitive to contamination by salts, RNases, detergents, and alcohol, all of which are typically used in commercial plasmid purification kits. As such, plasmids prepared by resin-based purification protocols must be further purified by phe-nol/chloroform and chloroform extraction. DNA should be precipitated with isopropanol, washed in ethanol, dried, and taken up in RNase-free water to a concentration of about 1 mg mL . The DNA should be stored frozen, in small aliquots. 

Surface isopropanol wash of the oily seats, followed by FTIR analysis, identified the residue as an aryl phosphate ester. The spectrum was compared with that of the flame retardant used in the seat material formulations (partially isopropylated triphenyl phosphate) and two matched very elosely. 

Crystd twice from toluene, washed with cyclohexane and dried at 60° under vacuum for several hours [Davis and Hetzer J Res Nat Bur Stand 60 569 1958]. Has also been recrystd from isopropanol and from diethyl ether/pet ether (b 40-60°). 

Rhodamine B chloride [3,5-his-(diethylamino)-9-(2-carboxyphenyl)xanthylium chloride] [81-88-9] M 479.0, m 210-211"(dec), Cl 45170, A,max 543nm, Free base [509-34-2] Cl 749, pK 5.53. Major impurities are partially dealkylated compounds not removed by crystn. Purified by chromatography, using ethyl acetate/isopropanol/ammonia (conc)(9 7 4, Rp 0.75 on Kieselgel G). Also crystd from cone soln in MeOH by slow addition of dry diethyl ether or from EtOH containing a drop of cone HCl by slow addition of ten volumes of dry diethyl ether. The solid was washed with ether and air dried. The dried material has also been extracted with benzene to remove oil-soluble material prior to recrystn. Store in the dark. 

Tetramethylammonium chloride [75-57-0] M 109.6, m >230°(dec). Crystd from EtOH, EtOH/CHCl3, EtOH/diethyl ether, acetone/EtOH (1 1), isopropanol or water. Traces of the free amine can be removed by washing with CHCI3. 

Sodium poly(a-L-glutamate). It was washed with acetone, dried, dissolved in water and ppted with isopropanol at 5°. Impurities and low molecular weight fractions were removed by dialysis of the aqueous solution for 50h, followed by ultrafiltration through a filter impermeable to polymers of molecular weights greater the 10. The polymer was recovered by freeze-drying. [Mori et al. J Chem Soc, Faraday Trans I 2583 1978.]... 

A mixture of 2.0 g (0.064 mol) of 2-fluoromethyl-3-(o-tolyl)-6-nitro-4(3H)-qulnazolinone, Oi g of 5% palladium-carbon and 100 ml of acetic acid is shaken for 30 minutes in hydrogen gas. The initial pressure of hydrogen gas is adjusted to 46 lb and the mixture is heated with an infrared lamp during the reaction. After 30 minutes of this reaction, the pressure of hydrogen gas decreases to 6 lb. After the mixture is cooled, the mixture is filtered to remove the catalyst. The filtrate is evaporated to remove acetic acid, and the residue is dissolved in chloroform. The chloroform solution is washed with 5% aqueous sodium hydroxide and water, successively. Then, the solution is dried and evaporated to remove solvent. The oily residue thus obtained is dissolved in 2 ml of chloroform, and the chloroform solution is passed through a column of 200 g of silica gel. The silica gel column is eluted with ethyl acetate-benzene (1 1). Then, the eluate is evaporated to remove solvent. The crude crystal obtained is washed with isopropylether and recrystallized from isopropanol. 0.95 g of 2-fluoromethyl-3-(o-tolyl)-6-amino-4(3H)-quinazolinone Is obtained. Yield 52.5% MP 195°-196°C. 

Introduce 33.6 g (0.2 mol) of 1,3 -trimethoxybenzene and 100 ml of chlorobenzene Into a 500 ml three-neck flask with stirrer, hydrochloric acid bubbler and condenser. Stir to dissolve and edd 27.7 g of 4-pyrro idinobutyronitrile (from 4hydrochloric acid gas in for 4 hours. Cool to about 5°C and add 200 cm3 of water, g ir. Decanttheaqueouslayer,wash again with 150cm3 of water. Combine the aqueous layers, drive off the traces of chlorobenzene by distilling 150 cm3 Qf water, and heat under reflux for one hour. Cool and render alkaline by means of 60 ml of sodium hydroxide solution of 36° Baume. Extract twice with 100 ml of ether. Wash the ether with 100 ml of water. Dry the ether over sodium sulfate and slowly run in 50 ml of 5N hydrogen chloride solution in ether, at the boil. Cool in ice. Filter, wash with ether and dry in a vacuum oven. 33.6 g of crude product are obtained. Recrystallize from 200 ml of isopropanol in the presence of 3 SA carbon black. Filter. Wash and dry in a vacuum oven. 

Then, 1-(3-acetylthio-2-methylpropanoyl)-L-proline is produced. The 1-(3-acetylthio-3-methyl-propanoyl)-L-proline tert-butyl ester (7.8 g) is dissolved in a mixture of anisole (55 ml) and trifluoroacetic acid (110 ml). After one hour storage at room temperature the solvent Is removed in vacuo and the residue is precipitated several times from ether-hexane. The residue (6.8 g) is dissolved in acetonitrile (40 ml) and dicyclohexylamine (4.5 ml) is added. The crystalline salt is boiled with fresh acetonitrile (100 ml), chilled to room temperature and filtered, yield 3 g, MP 187°C to 188°C. This material is recrystallized from isopropanol [ttlo -67° (C 1.4, EtOH). The crystalline dicyclohexylamine salt is suspended in a mixture of 5% aqueous potassium bisulfate and ethyl acetate. The organic phase is washed with water and concentrated to dryness. The residue is crystallized from ethyl acetate-hexane to yield the 1-(3-acetylthio-2-D-methylpropanoyl-L-proline, MP83°Cto 85°C. 

A mixture of 59.5 g of that oily product, 1.B5 liters of benzene and 1 kg of potassium bisulfite in 200 liters of water is stirred at room temperature for two hours. The precipitated bisulfite addition product of the ketone is isolated by filtration and washed with isopropanol and then with ether. Five hundred grams of the adduct is mixed with 119.5 g of potassium cyanide, 292 ml of B5% hydrazine hydrate and 910 ml of water. The mixture is stirred overnight at room temperature after which the product is isolated by filtration. The product is washed 3 times with 250 ml portions of water and then 3 times with 230 ml portions of ether. It is then air dried and vacuum dried at room temperature. The intermediate so produced has the following formula ... 

The mixture was stirred for 2 hours, heated at 60° to 70°C for 1 hour and poured into 2 liters of H O. The resulting suspension was extracted with ether, the ether layer separated and the ether removed under vacuum. A gummy mass remained which was dissolved in decalin and the solution was partly distilled to remove excess chlorobromide. After removal of most of the decalin under vacuum, the residue was treated with a large excess of N-( -hydroxyethyl)-piperazine and heated on a steam bath for 2 hours. This material was extracted with dilute aqueous HCI, this acid layer neutralized with aqueous base and the resulting oil extracted into ether. The ether layer was washed with water until the washings were neutral and dried over anhydrous potassium carbonate. On treatment with maleic acid in ether a yellow solid separated which was recrystallized from isopropanol. This yellow solid had MP 175° to 177°C. 

To a solution of 970 parts of 2,6-dihydroxyacetophenone and 325 parts of epichlorohydrin in 1,500 parts of hot isopropanol was added, with stirring under reflux, a solution of 233 parts of 85% KOH in 2,500 parts of isopropanol and sufficient water (ca 100 parts) to dissolve the solid. The mixture was heated, with stirring, under reflux for 48 hours. Half the solvent was then distilled off and 5,000 parts of water were added. The mixture was cooled and the solid filtered off and washed with isopropanol and ether. It was then recrystallized from 12,500 parts of isopropanol to obtain a first crop of 380 parts and a second crop, after concentration, of 300 parts of 1,3-bis(2-acetyl-3-hydroxyphenoxy)-2-hydroxypropane. 

Preparation of Alkaloid Mixture 50 ml of the concentrated benzene solution, obtained as described was rapidly stirred, and a saturated solution of hydrogen chloride in ether added to the concentrated benzene solution until no more precipitate was obtained. The resulting precipitate was recovered by filtration and comprised the crude hydrochlorides of the extracted alkaloids and the hydrochloride of any unrecovered triethylamine. This material was dried by heating at a temperature of about 75°C for 6 hours, the crude, dried precipitate ground with 50 ml of isopropanol and to this slurry was added 1,000 ml of water. The resulting mixture was filtered. To the clear filtrate, cooled to 5°C, there was slowly added with rapid stirring, a 10% aqueous solution of ammonium hydroxide, until complete precipitation was accomplished. The precipitate was filtered off, washed with water and dried by heating at about 75°C for 6 hours. 

The direct synthetic process is described in U.S. Patent 2,772,280. A solution of 73.3 g (0.332 mol) of (3-aminoxyalanine ethyl ester dihydrochloride in 100 ml of water was stirred in a 500 ml 3-necked round-bottomed flask cooled in an ice-bath. To the above solution was added over a 30-minute period 65.6 g (1.17 mols) of potassium hydroxide dissolved in 100 ml of water. While the pH of the reaction mixture was 7 to 10.5, a red color appeared which disappeared when the pH reached 11 to 11.5. The light yellow solution was allowed to stand at room temperature for 14 hour and then added to 1,800 ml of 1 1 ethanol-isopropanol. The reaction flask was washed twice with 10 ml portions of water and the washings added to the alcohol solution. The precipitated salts were filtered out of the alcohol solution and the filtrate cooled to 5°C in a 5 liter 3-necked round-bottomed flask. To the cold, well-stirred solution was added dropwise over a 35-minute period sufficient glacial acetic acid to bring the pH of the alcohol solution to 6.0. When the pH of the solution had reached 7 to 7.5, the solution was seeded and no further acetic acid added until Crystallization of the oil already precipitated had definitely begun. The crystalline precipitate was collected on a filter, washed twice with 1 1 ethanol-isopropanol and twice with ether. The yield of 4-amino-3-isoxazolidone was 22.7 g. 

The flask of a Parr hydrogenation apparatus was charged with 10,5 g of 3,3-diphenylpropyl-amine, 7.7 g of cyclohexylacetone, 50 ml methanol and 150 mg of platinum dioxide. Hydrogen at a pressure of 3 atmospheres was introduced and the mixture stirred. Upon absorption of the theoretical amount of hydrogen, stirring is discontinued, the catalyst is filtered off and the solution is evaporated to dryness. The residue is taken up with ether and the hydrochloride is precipitated with HCI in alcoholic solution. The product, as collected on a filter and washed with ether, is recrystallized from isopropanol. Yield 17 g (92.5% of theory). 

After 2 hours the mixture is cooled to about 0°C and the crude product Is collected by filtration, washed with diethyl ether and dried in a vacuum oven. After treatment with decolorizing charcoal and recrystallization from an equivolume mixture of isopropanol and methanol, the product, 2,5-bis(2,2,2-trifluoroethoxy)-N-(2-piperidylmethyl)benzamide hydrochloride has a MP of 228°C to 229°C. 

The reaction mixture is then warmed on the steam bath for an additional two hours (90°C to 95°C). The excess hydrazine hydrate is removed in vacuo. The residue of viscous 1-hy-drazlno-3-morpholinyl-2-propanol Is not distilled, but is mixed with 10.16 g (0.0B6 mol) diethyl carbonate and a solution of 0.3 g sodium metal in 15 ml methyl alcohol. The mixture is refluxed about 2 hours under a 15 cm Widmer column, the alcohol being removed leaving a thick, green liquid residue, which is cooled and the precipitate which forms is removed by filtration and washed well with ether. Yield B2%, MP114°C to 116°C. Recrystallization from isopropanol gives purified 3-amino-5-(N-morpholinyl)-methyl-2-oxazolidone, MP 120°C as the intermediate. 

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