Chloroform and acetone

LynestrenoL Lynestrenol (73) has been used in oral contraceptives and to treat menstrual disorders. It is converted in vivo to its active metabohte norethindrone (102,103). It can be recrystallized from methanol, and is soluble in ethanol, ether, chloroform, and acetone, and insoluble in water (102). The crystal stmcture (104) and other spectral and analytical data have been reported for lynestrenol (62). 

FIG. 13-12 Liq iiid boiling points and vapor condensation temperatures for maximum-boiling azeotrope mixtures of chloroform and acetone at 101.3 kPa (1 atm) total pressure. 

Cellulose for chromatography is purified by sequential washing with chloroform, ethanol, water, ethanol, chloroform and acetone. More extensive purification uses aqueous ammonia, water, hydrochloric acid, water, acetone and diethyl ether, followed by drying in a vacuum. Trace metals can be removed from filter paper by washing for several hours with O.IM oxalic or citric acid, followed by repeated washing with distilled water. 

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). 

Table I Thermo-oxidative stability (at 150 C) of PP (ICI.HF22) without and with 30X glass fibre (6F) in the absence and presence of antioxidants. Soxhlet extraction was with chloroform and acetone...

A mixture of tetracyanodibenzo-[l,4,7,10-tatrathia-12-crown] (1) (0.050 g, 0.115 mmol), 4-nitrophthalonitrile (2) (0.150 g, 0.690 mmol) and zinc(ll) acetate (0.050 g, 0.230 mmol) was refluxed in amyl alcohol under argon for 6 h (Scheme 42.1). The reaction mixture was cooled down to room temperature and precipitated by adding methanol. After filtration, the product was washed with methanol, chloroform and acetone. This compound was soluble in tetrahydrofuran (THF), dimeth-ylformamide (DMF) and dimethylsulfoxide (DMSO). 

Sulfur vaporizes at 444.6°C. The element, particularly in its orthorhombic Ss form, is insoluble in water but dissolves in carbon disulfide, anhydrous liquid ammonia, and methylene iodide. It is moderately soluble in benzene, toluene, chloroform, and acetone, solubility increasing with temperature. Solid polymeric sulfur is practically insoluble in all solvents. 

For example, in a general screen for acidic drugs, which includes most of the NSAIDs (Fig. 13.5), three mobile phases may be used. Table 13.3 shows the Rf values obtained for three NSAIDs in three different mobile phases. It can be seen from the data in Table 13.3 that even for closely related structures slight differences in polarity and lipophilicity can be exploited to produce separation. For instance, ibuprofen is the least polar drug in system 1 but is the most polar drug in system 3, where the carboxyl groups in the structures will be ionised due to the ammonia in the mobile phase. It can also be seen that the polarity of a mobile phase containing a mixture of chloroform and acetone is similar to that of pure ethyl acetate. 

PVAc has a specific gravity of 1.2 and an index of refraction of 1.47. It has a solubility parameter of 9.5 H and is soluble in liquids with similar solubility parameter values, such as benzene, chloroform, and acetone ... 

Some properties of these compounds that facilitate identification and assessment of purity are given in the Table I. All the compounds are air stable in the solid state as well as in solution. They are soluble in dichloromethane, acetonitrile, and nitromethane less soluble in chloroform and acetone, and insoluble in alcohols, ethers, and alkanes. The complex [RuC12(>/4-C8H12) (NCCH3)2] is also soluble in water. It may therefore have an extensive aqueous chemistry. 

Polyimides based on 3,5-diaminodiphenylsulfide demonstrate that solubility in organic solvents strongly depends on the nature of the dianhydride used polymers based on dianhydride 6F and dianhydride A are soluble in NMP, chloroform and acetone polyimides based on diphenyloxide-3,3, 4,4 -tetracarboxylic and benzophenone-3,3, 4,4 -tetracarboxylic acid dianhydrides are soluble in NMP only. Polyimides demonstrate high aired NMP (0.79-1.20 dl/g) and moderate (210-250 °C) Tg values combined with high (400-460 °C) T egr-... 

Desmaroux has also determined the nitroglycerine absorption isotherms from its chloroform and acetone solutions at 20°C by a nitrocellulose with a nitrogen content of 11.2-13.35 and 14.2% N (Figs. 94a and 94b respectively) as well as those of nitro-glycol in an ethyl ether solution at 20°C sorbed by nitrocellulose of 12.2% N as shown in Figs. 95a and 95b. 

Figure 13.23. Examples of vapor-liquid equilibria in presence of solvents, (a) Mixture of-octane and toluene in the presence of phenol, (b) Mixtures of chloroform and acetone in the presence of methylisobutylketone. The mole fraction of solvent is indicated, (c) Mixture of ethanol and water (a) without additive (b) with 10gCaCl2 in 100 mL of mix. (d) Mixture of acetone and methanol (a) in 2.3Af CaCl2 ip) salt-free, (e) Effect of solvent concentration on the activity coefficients and relative volatility of an equimolal mixture of acetone and water (Carlson and Stewart, in Weissbergers Technique of Organic Chemistry IV, Distillation, 1965). (f) Relative volatilities in the presence of acetonitrile. Compositions of hydrocarbons in liquid phase on solvent-free basis (1) 0.76 isopentane + 0.24 isoprene (2) 0.24 iC5 + 0.76 IP (3) 0.5 iC5 + 0.5 2-methylbutene-2 (4) 0.25-0.76 2MB2 + 0.75-0.24 IP [Ogorodnikov et al., Zh. Prikl. Kh. 34, 1096-1102 (1961)].

Low-wavelength UV detection (200-210 nm) is more sensitive and permits the use of gradients but precludes the use of certain common lipid solvents, such as chloroform and acetone, which are opaque in the UV region of interest. With low-wavelength UV detection, the response will also be somewhat dependent on fatty acid composition. For these reasons the mobile phases used in lipid analysis by HPLC may seem rather strange to workers familiar with the Thin Layer Chromatography (TLC) or open column separations. 

The sample diluent affects the solute dispersion. If we consider the effects of three different diluents (hexane, chloroform, and acetone) on the chromatographic behavior of a TG mixture on RP columns using, for example, acetonitrile and ethanol as the mobile phase, we can see that the TGs dissolved in hexane provided only a minute chromatographic trace, whereas dissolution in chloroform yielded excellent detection and resolution. These results can best be explained by invoking the solvophobic theory of Horvath and Melander (85). 

All of the B2 vitamers are unstable at alkaline pH the coenzymes are also degraded below pH 5.0 (80 - 82). As a result, analysis of the endogenous coenzymes needs to be carried out at pH 5.0-7.0, while total riboflavin (as riboflavin) is best determined at acidic pH. Riboflavin is soluble in water and short-chain alcohols, but insoluble in ether, chloroform, and acetone. The coenzymes are water soluble. 

At 200°C or above, at atmospheric pressure, however, the range of solvents is limited. High-boiling solvents also are inconvenient to remove and to re-purify. These aspects militate against (but do not rule out) the use of MORE chemistry for scale-up beyond the hundreds of gram. On the other hand, temperatures in the order of 200°C can be attained at pressures of 2-3 MPa for solvents such as ethyl acetate, methanol, ethanol, acetonitrile, chloroform and acetone, all of which boil below 85°C at ambient pressure. 

Acetone and Alkali. In the presence of potassium hydroxide or calcium hydroxide, chloroform and acetone react vigorously to form l,l,l-trichloro-2-hydroxy-2-methylpropane.2-4... 

Example 1. Partial pressures of chloroform and acetone solutions (in torr at 35.2°C) above a solution of these components are given below. Calculate the Raoult s law reference activity coefficients for each component at each composition. 

In systems with negative deviation from ideal behavior, maximum-boiling-point azeotropes can occur. This is illustrated in Fig. 8 for the chloroform-acetone system, treated in Example 1. This system shows negative deviation from ideal behavior due to the possibility of hydrogen bonds between chloroform and acetone, which cannot occur with the pure components. 

Adsorption of y-Aminopropyltrimethoxysilane onto the Polypropylene Film. The reaction with y-aminopropyltri-methoxysilane was performed using 2% v/v toluene solution under N2 atmosphere for 16 hours. The film was successively washed with toluene, chloroform, and acetone. Then the film was washed with water for half an hour. Finally, methanol washing was performed and the film was dried. 

Further evidence for the hypothesis was found in the patent describing the isoprene—acrylonitrile—zinc chloride system (23). On adding a four-fold excess of isoprene to an equimolar mixture of acrylonitrile and zinc chloride, in the absence of a free radical catalyst, an exothermic reaction occurs after approximately 30 minutes. The recovered polymer is insoluble in hydrocarbons, chloroform, and acetone. This eliminates polyisoprene and the alternating copolymer. The yield of product is 12%, calculated a polyacrylonitrile, compared with the 16.8% yield of copolymer obtained when excess acrylonitrile and a free radical catalyst are used. 

Purified fucoxanthin Brown seaweed Normal phase, silica gel column Chloroform and Acetone (9 1) isocratic Yan et al., 1999... 

This salt is soluble in water, but is insoluble in alcohol, ether, chloroform, and acetone. 

Calculate the activity coefficients of chloroform and acetone at 0°C in a solution containing 50 mol % of each component, using the Wilson-equation model. The Wilson constants for the system (with subscript 1 pertaining to chloroform and subscript 2 to acetone) are... 

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