Of isopropanol

Collision-induced dissociation mass spectrum of tire proton-bound dimer of isopropanol [(CH2)2CHOH]2H. The mJz 121 ions were first isolated in the trap, followed by resonant excitation of their trajectories to produce CID. Fragment ions include water loss mJz 103), loss of isopropanol mJz 61) and loss of 42 anui mJz 79). (b) Ion-molecule reactions in an ion trap. In this example the mJz 103 ion was first isolated and then resonantly excited in the trap. Endothennic reaction with water inside the trap produces the proton-bound cluster at mJz 121, while CID produces the fragment with mJz 61. 

When aldehydes or ketones are heated with an excess of isopropanol in the... 

Place in the flask 2 g. of benzophenone, 15 ml. of isopropanol and 2 5 g. of aluminium isopropoxide. This mixture has now to be heated gently under reflux so that the temperature registered by the thermometer in the column does not exceed 80°, i.e., so that only acetone distils. For this purpose, the flask should preferably be heated in an oil-bath direct heating, even over an asbestos sheet, may cause local overheating and decomposition the use of a water-bath on the other hand may make the column undesirably damp. 

Place 38 ml. of isopropanol in a two-necked 500 ml. round-bottomed flask fitted with (a) a reflux water-condenser having a calcium chloride tube at the top, and (b) a dropping-funnel. Cool the flask in ice-water and then run 13 5 ml. of phosphorus trichloride in from the dropping-funnel during 15 minutes. Then allow the reaction-mixture to attain room temperature. Now replace the condenser and the... 

Alkylation of 2-methylaminothiazole (204) with ROH in 85% sulfuric acid gives 2-methylimino-3-alkyl-4-thiazoIine (54). 2-Amino-4-rnethyl-thiazoie alkylated with an excess of isopropanol, however, gives 95% of 2-isopropylamino-4-methyl-5-isopropylthiazole (56). The same result is obtained with cyclohexanol (242). These results and those reported in Sections III.l.C and IV.l.E offer interesting new synthetic possibilities in thiazole chemistry. The reactive species in these alkylations is the conjugate acid of 2-aminothiazole. and the diversity of the products obtained suggests that three nucleophilic centers may be operative in this species. 

C. Sbeely, Jr., Kinetics of Cataljtk Dehydrogenation of Isopropanol, University Microfilms, Arm Arbor, Michigan, 1953, p. 3. 

Eyrol 51 is a water-soluble Hquid containing about 21% phosphoms. It is made by a multistep process from dimethyl methylphosphonate, phosphoms pentoxide, and ethylene oxide. The end groups are principally primary hydroxyl and the compound can thus be incorporated chemically into aminoplasts, phenoHc resins, and polyurethanes. Eyrol 51, or 58 if diluted with a small amount of isopropanol, is used along with amino resins to produce a flame-retardant resin finish on paper used for automotive air filters, or for backcoating of upholstery fabric to pass the British or California flammabiHty standards. 

Dehydration The growing use of isopropanol as a clean-rinse fluid in microelectronics produces significant quantities of an 8.5-90 percent isopropanol waste. Removing the water and trace contan ii-nants is required before the alcohol can be reused. Pervaporation produces a 99.99 percent alcohol product in one step. It is subsequently polished to remove metals and organics. In Europe, dehydration or ethanol is the largest pei vaporation application. For the very large ethanol plants typical of the United States, pei vaporation is not competitive with thermally integrated distillation. 

For maintenanee of optimum values pH at definition of Rh and Ir used the aeetie buffer mixes, prepared with addition of isopropanole. Colour of eomplexes develops within 2 h at 65 5°C or during 5 min under influenee of mierowave radiation. 

Purified by recrystn from aqueous EtOH or MeOH or aqueous NH3 + EtOH or isoPrOH. Also recrystd from aqueous ammoniacal soln at pH 10.5 (lOOmg/mL) by diluting with 5 volumes of isopropanol and then adjusting to pH 6 with acetic acid. An aqueous soln buffered to pH 10 with Na2C03 can be stored in a refrigerator for 1 week without decomposition. UV Xma, 226nm (/ij 4.02). The tartrate salt has m 165-166° (dec), 166-168° (dec), and [ag -41° (c 0.7, H2O). [Stammer et al. J Am Chem Soc 79 3236 7959 UV Kuehl J Am Chem Soc 77 2344 7955.]... 

SynChropak GPC supports can be packed by slurrying in methanol and packing upward with methanol to a pressure of 4000 psi. SynChropak CATSEC supports can be packed by slurrying in a mixture of isopropanol and methanol and packing upward with methanol to a pressure of 4000 psi. The high pore... 

Titrimetric analysis is a classical method for generating concentration-time data, especially in second-order reactions. We illustrate with data on the acetylation of isopropanol (reactant B) by acetic anhydride (reactant A), catalyzed by A-methyl-imidazole. The kinetics were followed by hydrolyzing 5.0-ml samples at known times and titrating with standard base. A blank is carried out with the reagents but no alcohol. The reaction is... 

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 reaction product (1-carbethoxymethyM-carbomethoxy-pyridinium bromide) was obtained in crystalline form. (It formed prisms melting at 166°-169°C after recrystallization from a mixture of isopropanol and acetone.) It was not necessary to isolate it. For the following reduction step, the reaction mixture was brought into solution by the addition of about 1 liter of warm ethyl alcohol. It was then hydrogenated at about 30 atm pressure in the presence of 2 g of platinum oxide. The temperature rose during this reaction to about 40°C. 

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. 

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. 

A mixture of 5.0 g of 3-chloro-5-(3-chloropropyl)-10,11 -dihydro-5H-dibenz(b,f)azepine, 5.0 g of 4-carbamoyl-4-piperidinopiperidine and 50 mi of dimethylformamide is heated at 100°C for 10 hours. The solvent is distilled off. After the addition of a 2% sodium carbonate solution to the flask, the content is scratched to yield a semisolid, which is dissolved in 50 ml of isopropanol. A solution of 5 g of maleic acid in 50 ml of isopropanol is added, and the precipitate is collected by filtration and recrystallized from isopropanol to give 5.6 g of crystalline 3-chloro-5-[3-(4-carbamoyl-4-piperidino-piperidino)propy I] -10,1 l-dihydro-SH-dibenz-Ib.fjazepine dilhydrogen maleate) with 1/2 molecule of water of crystallization melting at 181°C to 183°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. 

On evaporation of the ethyl ether from the ethyl ether solution, the benzhydryl ether was recovered as a pale yellow oil. The benzhydryl ether was dissolved in 60 ml of isopropanol and the isopropanol solution acidified to a pH of 3 with dry hydrogen chloride-methanol solution. The acidic propanol solution was then diluted with ethyl ether until a faint turbidity was observed. In a short time, the crystalline hydrochloride salt of the benzhydryl ether separated from the propanol solution. The crystallized salt was recrystallized once from 75 ml of isopropanol with the aid of ethyl ether in order to further purify the material. A yield of the pure hydrochloride salt of 1-methylpiperidyl-4-benzhydryl ether of 24.5 grams was obtained. This was 39% of the theoretical yield. The pure material had a melting point of 206°C. 

A sample of distilled base in cold isopropanol is treated with excess methyl iodide, left at room temperature overnight, diluted with 5 volumes of ethyl acetate and filtered from the methiodide salt. This is purified by crystallization from mixtures of isopropanol and ethyl acetate, filtering hot to remove an impurity of low solubility. The pure methiodide is obtained as a white solid, MP 124° to 124.5°C, containing 99 mol percent thiol isomer. 

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 filtrate is evaporated under vacuum and the residue is crystallized from a solution of 60 parts of isopropanol in 75 parts of water. There are obtained 9 parts of N-(3-sulfamyl-4-chlorobenzamido)-2-methyl indoline, MP (K) 184° to 186°C, MP (MK) 160° to 162°C (isopropanol/water). [The melting points being determined on a Kofler heater plate under the microscope (MK) or on a Kofler Bank (K)]. ... 

The free base d(-f)6-phenyl-2,3,5,6-tetrahydroimida2o[2,1-bl thiazole Is dissolved in 112 ml of acetone and 178 ml of isopropanolic hydrogen chloride is added all at once. The hydrochloride crystallizes et once. After cooling to below 0°C, the salt is recovered by filtration and washed with acetone. The product weighs 75.2 g (0.312 mol), 91%, from the camphor-sulfonate, melting point 227 C to 227.5°C [alpM-H23.1°C (C = 15.H20). 

To a solution of 18.9 grams (0.166 mol) n-heptaldehyde in 25 ml of isopropanol is added, with stirring, a solution of 19,1 grams (0.166 mol) of 1-aminohydantoin in 110 ml water acidified with concentrated HCI. The heavy white precipitate formed is filtered and washed, until acid free, with small amounts of water and ether. The yield of N-(n-hBptylidenB)-1-aminohydantoin is 14 grams of MP 150°C (with decomposition). This may be recrystal-lized from dimethylformamide. 

B.5 parts of 1 -azaphenothiazine carboxylic acid chloride and 14 parts of piperidino-ethoxy-ethanol were introduced into 100 parts of chlorobenzene and the mixture boiled under reflux for 5 minutes. After cooling off the precipitated hydrochloride salt of piperidino-ethoxy-ethanol was filtered off on a suction filter. Water was added to the filtrate and the pH thereof adjusted to 5 to 6 with dilute HCI. The aqueous phase was then removed, a caustic soda solution added thereto and then extracted with ether. The ethyl extract waswashed with water, then dried with potash and the ether distilled off. 9.4 parts of the piperidino-ethoxy-ethyi ester of 1 -azaphenothiazine carboxylic acid were obtained. This product was dissolved in 20 parts of isopropanol and the solution neutralized with isopropanolic HCI. The monohydrochloride which precipitated out after recrystallization from isopropanol had a melting point of 160°Cto 161°C. 

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%. 

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