Subject acetone mixture

A mixture of 4.98 g of acetoacetic acid N-benzyl-N-methylaminoethyl ester, 2.3 g of aminocrotonic acid methyl ester, and 3 g of m-nitrobenzaldehyde was stirred for 6 hours at 100°C in an oil bath. The reaction mixture was subjected to a silica gel column chromatography (diameter 4 cm and height 25 cm) and then eluted with a 20 1 mixture of chloroform and acetone. The effluent containing the subject product was concentrated and checked by thin layer chromatography. The powdery product thus obtained was dissolved in acetone and after adjusting the solution with an ethanol solution saturated with hydrogen chloride to pH 1 -2, the solution was concentrated to provide 2 g of 2,6-dimethyl-4-(3 -nitrophenyl)-1,4-dihydropyridlne-3,5-dicarboxylic acid 3-methylester-5- -(N-benzyl-N-methylamino)ethyl ester hydrochloride. The product thus obtained was then crystallized from an acetone mixture, melting point 136°Cto 140°C (decomposed). 

One of the earliest reported preparations of the requisite glycosidation precursor 5-deoxy-l,2,3-tri-0-acetyl-p-D-ribofuranoside (17) was published by Kissman and Baker in 1957.23 D-Ribose was heated at reflux in a methanol/acetone mixture in the presence of concentrated HCI to provide methyl 2,3-O-isopropylidene-D-ribofuranosidc (21), which was in turn converted to the corresponding 5-O-mesyl ribofuranoside 22 with methanesulfonyl chloride in pyridine in 63% yield. The sulfonate moiety of 22 was then displaced with sodium iodide in refluxing DMF to provide 5-deoxy-5-iodo derivative 23 in 76% yield on a multigram scale. Reductive dehalogenation of 23 was accomplished under heterogeneous catalytic hydrogenation conditions to provide the reduced 2,3-0-protected intermediate 24 in 56% yield, which was subjected to hydrolysis conditions in... 

In the laboratory of R. Bihovsky, a series of peptide mimetic aldehyde inhibitors of calpain I was prepared in which the P2 and P3 amino acids were replaced with substituted 3,4-dihydro-1,2-benzothiazine-3-carboxylate-1,1-dioxides. The synthesis began with the diazotization of the substituted aniline substrate using sodium nitrite and hydrochloric acid. The aqueous solution of the corresponding diazonium chloride product was added dropwise to the solution of acrylonitrile in a water-acetone mixture, which contained catalytic amounts of copper(ll) chloride. This Meerwein arylation step afforded the chloronitrile derivative, which was subjected to sulfonation with chlorosulfonic acid, and the resulting sulfonyl chloride was treated with the solution of ammonia in dioxane to give the desired 3,4-dihydro-1,2-benzothiazine-2-carboxamide. 

Fig. 6. Gel electrophoresis of the outer and the cytoplasmic membrane pulse labeled for 10 seconds with [ H]arginine. E. coli MX74T2 was labeled with 2.5 /iCi [ CJarginine for 1.5 h. Then 50 lCi [ H]arginine was added to the culture, and the mixture was incubated for 10 sec. Immediately after the pulse label, the culture was cooled in a dry ice-acetone mixture. The outer and inner membrane fractions were separated and then subjected to SDS gel electrophoresis. (A) The outer membrane. (B) The cytoplasmic membrane. [ C]arginine ------- ...

I have found that a mixture of citral and acetone, if it is subjected, in the presence of water, for a suffieiently long time to the action of hydrates of alkaline earths or of hydrates of alkali metals, or of other alkaline agents, is eondensed to a ketone of the formula CjjH pO. This substanee, which I term Pseudo-ionone," may be produced lor instance in shaking together for several days equal parts of citral and acetone with a solution of hydrate of barium, and in dissolving the products of this reaction in ether. 

The process for the production of the pseudo-ionone referred to in the first claim, consisting in the subjection of a mixture of citral and acetone to the action of an alkaline agent, and in purifying the product of this reaction, extracted by means of ether, by fractional distillation, substantially as described. 

IC-0 residue is cleaned up with a mixture of dichloromethane and acetone by liquid-liquid partitioning under neutral conditions and then extracted into diethyl ether under acidic conditions. The diethyl ether in the extract is removed by rotary evaporation and the residue is dissolved in buffer solution, which is subjected to a cleanup procedure using a Sep-Pak Cig Env. column. 

In a related approach from the same laboratory, the perfluorooctylsulfonyl tag was employed in a traceless strategy for the deoxygenation of phenols (Scheme 7.82) [94], These reactions were carried out in a toluene/acetone/water (4 4 1) solvent mixture, utilizing 5 equivalents of formic acid and potassium carbonate/[l,T-bis(diphe-nylphosphino)ferrocene]dichloropalladium(II) [Pd(dppf)Cl2] as the catalytic system. After 20 min of irradiation, the reaction mixture was subjected to fluorous solid-phase extraction (F-S PE) to afford the desired products in high yields. This new traceless fluorous tag has also been employed in the synthesis of pyrimidines and hydantoins. 

The mutual solubility Of two salts.—Numerous investigations have been made on this subject in the light of the phase rule by H. W. B. Roozeboom 8 and others. C. E. Linebarger also submitted mixtures of two salts to the action of various organic liquids in which one of the salts was insoluble. If both salts passed into soln. in a molecular ratio, it was assumed that a double salt is formed in soln. With a mixture of sodium and mercuric chlorides no double salt was formed with benzene or acetone as solvent, but with acetic ether, a salt, (HgCl2)2NaCl, was formed similarly also with lithium and mercuric chlorides, the salt HgCl2.LiCl was formed but no double salt was observed with potassium and mercuric chlorides in the same solvent. 

Does the amount of acetone increase, decrease, or remain the same when an equilibrium mixture of reactants and products is subjected to the following changes ... 

To a solution of aldimine 1 (0.01 mol) in acetone, added ethyl-a-mercapto/a-cya-noacetate (0.01 mol) followed by basic alumina (20 g) with constant stirring. The reaction mixture taken in a beaker, was thoroughly mixed and the adsorbed material was dried in air. The adsorbed reactant in the beaker was placed in an alumina bath and subjected to microwave irradiation for 1-2 min. On completion of the reaction as followed by TLC examination, the mixture was cooled to room temperature and the product was extracted into acetone (3x15 mL). Recovering of solvent under reduced pressure yielded the product, which was purified by recrystallization from the mixture of ethanol-acetone. 

A mixture of substituted 2 -hydroxychalcone (1 mmol), the corresponding support (5 g) and the additive (5 mg) in a Pyrex tube was subjected to irradiation at 45 W for 20 min in a Maxidigest 350 Prolabo monomode, focused microwave (2.45 GHz) reactor with continuous rotation. The cooled mixture was washed with methylene chloride (2xl0mL) and concentrated in vacuo. The residue was purified by two subsequent column chromatographies (silica gel) by using hexane-acetone (4 1, v/v) and toluene or toluene-ethyl methyl ketone (30 1, v/v) as eluent. 

Method for diamines and poly amines by HPLC. To a mixture of one volume of amine solution (less than 1 nmole/pl) is added an equal volume of 0.1 M borate buffer (pH 8.0) [101]. The solutions are mixed and one volume of fluorescamine solution (20 mg/10 ml in acetone) is added with rapid shaking using a vortex mixer or the equivalent. An aliquot portion of this mixture is then subjected to chromatography for separation and analysis. 

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