Isopropanol, Anhydrous

Separation of isopropanol (IPA) and water by pervaporation has also reached production scale. Much of the current capacity is devoted to azeotrope breaking and dehydration during IPA synthesis. Recently, anhydrous isopropanol has become a preferred drying solvent in the semiconductor industry, where chip wafers are first washed with ultrapure water, then rinsed with the alcohol to promote uniform drying. The water-laden isopropanol generated can be conveniently reused after dehydration by pervaporation. Unlike with pressure-driven membrane processes such as RO or UF, particulates and nonvolatile substances such as salts are not carried over during pervaporation. This helps maintain the effectiveness of contamination control. 

After each filter is scanned the crystal may require cleaning. Due to the toxicity of the KRS-5 crystal, it is left in the crystal holder at all times so as to avoid unnecessary handling as well as, scratching or damaging the crystal. The crystal, in its holder, is flushed with a forced stream of anhydrous isopropanol from a plastic wash bottle. A cotton swab, soaked in isopropanol, can be used to remove deposits on the crystal. This should be done with very light rubbing as the KRS-5 crystal scratches very easily. 

MTT solubilization solution 10% Triton X-100 in O.IN hydrochloric acid in anhydrous isopropanol (solution can be stored at room temperature 15-25°C). 

Grafting of Al on SBA-15 was performed from Al isopropoxide, Al(0-iPr)3 (Aldrich). This compound was dissolved in 20 mL of either anhydrous isopropanol (Fluka) or anhydrous cyclohexane (Fluka) before suspending the SBA-15 support previously dehydrated for 2h at 450°C. In order to avoid the presence of any traces of water the reaction was performed in Ar atmosphere. The suspension was left under stirring overnight before filtration and washing with the corresponding anhydrous solvent. The solid was then calcined at 500°C for 4h. This material corresponds to the grafting. The whole procedure was... 

In a 2-liter, resin kettle equipped with a mechanical stirrer, reflux condenser, thermometer, and a means of maintaining the reaction mixture under a nitrogen atmosphere, a solution of 886 gm of diallyl o-phthalate, 62.2 gm of anhydrous isopropanol, and 7.5 gm of 50.4% hydrogen peroxide is heated with stirring, under nitrogen at reflux (104°-108°C) for 10 hr. At the end of this time, the viscosity of the reaction mixture, at 106°C, is 27 cPs. 

The reaction mixture is cooled to 25°C whereupon the viscosity of the solution is found to be 425 cPs. The reaction mixture is added with cooling to 5 liters of anhydrous isopropanol which has been cooled to 0°C. The prepolymer, which precipitates, is filtered off and dried under reduced pressure (yield 245 gm 27.6%). The umeacted monomer may be recovered from the filtrates. 

Exemplary catalyst can be prepared by using isopropanol dried with nitrogen. In the anhydrous isopropanol, calcium acetate is dissolved at a temperature of 105°C. The obtained catalyst is modified by using sulfuric acid (molar ratio of calcium acetate to sulfuric acid is equal to 2). Volatile components (water, isopropanol, and acetic acid) are then distilled under decreased pressure. 

It is advisable in any case before an experiment to place the weighed aluminium isopropoxide overnight in a shallow dish in a vacuum desiccator over sodium hydroxide. The isopropanol should be dried over anhydrous sodium sulphate, and the clear liquid decanted off before use. 

The U.S. domestic shipping name of isopropyl alcohol is UN No. 1219 Isopropanol. Anhydrous as well as water solutions to 91 vol % alcohol are considered flammable Hquid materials by the DOT. Both have flash poiats below 37.8°C by the Tag closed-cup method. Acceptable modes of transportation include air, rail, road, and water (124). For international air and water shipments, the International Maritime Organization (IMO) class is 3.2, the packaging group is II, and the primary hazard label required is "Flammable Liquid."... 

To a solution of 1.0 g (0.003 mole) of iridium tetrachloride in 0.5 ml of concentrated hydrochloric acid is added 15 ml of trimethylphosphite. This solution is added to a solution of 7.7 g (0.05 mole) of 4-/-butylcyclohexanone in 160 ml of isopropanol in a 500-ml flask equipped with a reflux condenser. The solution is refluxed for 48 hours, then cooled, and the isopropanol is removed on a rotary evaporator. The residue is diluted with 65 ml of water and extracted four times with 40-ml portions of ether. The extracts are dried with anhydrous magnesium sulfate, filtered, and the ether is removed on the rotary evaporator. The white solid residue is recrystallized from 60 % aqueous ethanol affording cis alcohol of greater than 99% purity, mp 82-83.5°. 

The product Is often used as the acid sulfate which is produced as follows 252.0 g (0.B5 mol) of 0 A-diphenyl-7-dlmethylamlnovaleramide was dissolved in one liter of isopropanol,and 70 ml of concentrated sulfuric acid was added as rapidly as possible. The mixture was heated until clear, then filtered and diluted with 1,500 ml of anhydrous ethyl acetate. The solution was cooled and filtered, and the white crystalline product was dried in vacuo over PjOs. 

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. 

The product was dissolved in isopropanol, and the solution was acidified with anhydrous hydrochloric acid, yielding the hydrochloride, MP 206°C to 208°C (decomp.). 

On the addition of ethereal hydrogen chloride to a solution of the base in isopropanol and recrystallization from anhydrous ethanol of the salt formed, there is obtained 3-dimethyl-sulfamovl-10-(2-dimethvlaminopropyl)phenthiazine hydrochloride (2.1 grams), MP 214°C with decomposition. After dissolving the product in anhydrous ethanol and adding meth-anesulfonic acid there is obtained fonazine mesylate. 

After cooling, the reaction mixture is agitated (with a mixture of (water (40 cc) and a normal solution of methanesulfonic acid (70 cc), the xylene layer is removed and the acid liquors are (washed (with ether (200 cc). The aqueous phase is then made alkaline (with sodium hydroxide (d = 1.33 10 cc) and the liberated base Is extracted (with ether. The ethereal solution is dried over anhydrous potassium carbonate and concentrated at normal pressure. On distillation of the residue under reduced pressure 3-(3-methoxy-10-phenthi-azinyl)-2-methyl-1-dimethylaminopropane (11.3 g) is obtained, MP 103°C, BP 182° to 191°C/0.15 mm Hg. The hydrochloride prepared in isopropanol melts at about 90°C. 

The mixture was heated under reflux and a solution of 0.2 g of ethyl iodide in 5 ml of dry tetrahydrofuran was allowed to flow into the reaction medium. When the reaction started, a solution of 6.2 g of 7heated under reflux until the complete disappearance of the magnesium turnings. The reaction medium was then cooled in an ice bath, after which there was added thereto a solution in 45 ml of tetrahydrofuran of 7 g of 6-oxo-benzo[b] -benzofurano[2,3-e] oxepin. The reaction mixture was allowed to stand for 20 hours at a temperature of 20°C, and was then poured into a saturated aqueous solution of ammonium chloride maintained at a temperature of 5°C. The mixture was extracted with ether and the organic portion was washed and dried over anhydrous sodium sulfate. After evaporation of the solvent, 9.4 g of crude product were obtained, which after recrystallization from isopropanol, provided 6.7 g of pure 6-(3-dimethylam nopropyl)-8-hydroxybenzo[b] benzofurano-[2,3-e] oxepin, melting point 160°C (yield, 71 %). 

To obtain the free base, 34 g (0.256 mol) of N-ethyl-3-piperidinol and 20 g (0.22 mol) of diphenylacetyl chloride were mixed in 80 cc of isopropanol and the solution was refluxed for 2 hours. The isopropanol was evaporated in vacuo at 30 mm pressure, the residue was dissolved in 150 cc of water and the aqueous solution was extracted several times with ether. The aqueous solution was then neutralized with potassium carbonate and extracted with ether. The ethereal solution was dried over anhydrous potassium carbonate and the ether removed by distillation. The product was then distilled at its boiling point 180° to 181°C at 0.13 mm of mercury whereby 14 g of a clear yellow, viscous liquid was obtained. The nitrogen content for CjiHjjNOj was calculated as 4.33% and the nitrogen content found was 4.21%. 

The reaction mixture is chilled, diluted with anhydrous ether and the quaternary salt thus precipitated is collected on a filter and washed with dry ether and then with butanone. (3-Diisopropylaminoethyl xanthene-9-carboxylate methobromide thus obtained melts at 152°-153°C. After recrystallization from isopropanol it melts at 157°-155°C. 

The oil wes extracted with ether, the ether solution dried with anhydrous magnesium sulfate, and then filtered. Dry hydrogen chloride was passed into the ether solution and a semisolid mass, which crystallized after scratching, separated therefrom. The crude N-(j -pyrrolidino-ethyD-phenothiazine was separated from the ether and, after two crystallizations from isopropanol, 17.0 g of desired product, melting at 196°C to 197°C (uncorr.), was obtained. 

This treatment is continued until the /3-diethylaminoethyl chloride disappears (TLC). The oil is then dissolved in isopropanol and weakly acidified w h HCI in propanol. The 2/3-N-diethyl-aminoethylthio-4-p-phenylthiophenyl-3H-1,5-benzodlazepine HCI product crystallizes by addition of anhydrous ethyl ether to the solution. The crystals are filtered and recrystallized from ethyl acetate. Yield 3.65 g, melting point 150°C. 

The resulting solution is poured into ice acidified with dilute hydrochloric acid. A white solid precipitates which Is extracted into ether. The ether phase is washed with a saturated solution of sodium chloride and dried over anhydrous magnesium sulfate. The solvent is evaporated and a white solid, 5-(p-toluoyl)-1 -methylpvrrole-2-acetic acid is obtained which is recrystal-lized twice from isopropanol, melting point 155°C to 157°C. 

In 1906, Matignon reported an enthalpy of solution of -21.54 kcal mol-1 (-90 kj mol ) for neodymium trichloride in ethanol (178). His ethanol may have been less than perfectly anhydrous, and the value for pure ethanol somewhat less negative than this, perhaps —80 or — 70 kJ mol 1. Certainly a value in this region is considerably less negative than his value for the enthalpy of solution of neodymium trichloride in water, —148 kj mol-1. The difference may reasonably be attributed to less favorable solvation qf the constituent ions in ethanol than in water. Ion solvation would be expected to be even less favorable in isopropanol, so it is not surprising to find an enthalpy of solution of about + 40 kJ mol-1 for neodymium trichloride in this alcohol. This estimate must be considered as only approximate, as it is derived from... 

Friedel-Crafts alkylations can be carried out with isopropanol using anhydrous BF3 as an active catalyst. 

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