Tris carbon tetrachloride

Geranyl chloride can be prepared from geraniol by the careful use of triphenylphosphine in carbon tetrachloride. Tris(dimethylamino)phosphine reacts with carbon tetrachloride to form the complex (42) which can be used to form the enol esters (43) from acid anhydrides. Similarly, aldehydes form the alkenes (44), and esters or amides of trichloroacetic acid are converted to glycidic esters. ... 

Among the procedures tried were thionyl chloride and pyridine, phosphorus pentachlo-ride, triphenyiphosphine dibromide in N, N-dimethylformamide, triphenylphosphine and carbon tetrachloride, tris(dimethylamino)phosphine and bromine, o-phenylenephosphoro-chloridite and bromine, tris(dimethylamino)phosphine and carbon tetrachloride, and tri-n-octylphosphine and carbon tetrachloride. 

Thallium(III) trifluoroacetate. Tri-phenylphosphine-Carbon tetrachloride. Tris(triphenylphosphine) chlororhodium. 

Also, Kotani et al. [437] reported using controlled/ livmg atom transfer radical polymerization (ATRP) to form block copolymers of ethyl and n-butyl methacrylates. A ternary initiating system that consists of carbon tetrachloride, tris(triphenyl-phosphine)ruthenium dichloride [RuCl2(PPh3)3], and aluminum compounds produced ABA triblock copolymers [437]. 

Chlorinated by-products of ethylene oxychlorination typically include 1,1,2-trichloroethane chloral [75-87-6] (trichloroacetaldehyde) trichloroethylene [7901-6]-, 1,1-dichloroethane cis- and /n j -l,2-dichloroethylenes [156-59-2 and 156-60-5]-, 1,1-dichloroethylene [75-35-4] (vinyhdene chloride) 2-chloroethanol [107-07-3]-, ethyl chloride vinyl chloride mono-, di-, tri-, and tetrachloromethanes (methyl chloride [74-87-3], methylene chloride [75-09-2], chloroform, and carbon tetrachloride [56-23-5])-, and higher boiling compounds. The production of these compounds should be minimized to lower raw material costs, lessen the task of EDC purification, prevent fouling in the pyrolysis reactor, and minimize by-product handling and disposal. Of particular concern is chloral, because it polymerizes in the presence of strong acids. Chloral must be removed to prevent the formation of soflds which can foul and clog operating lines and controls (78). 

The submitters report that both l,4-diazabicyclo[2.2.2]octane and triethylamine have been used to catalyze this decomposition. Tri-ethylamine was less satisfactory as a catalyst because of its relatively rapid reaction with the solvent, carbon tetrachloride, to form triethylamine hydrochloride and because of difficulty encountered in separating triethylamine from the dicarbonate pi oduct. The 1,4-diazabicyclo-[2.2.2]octane was efficiently separated from the dicarbonate product by the procedure described in which the crude product was washed with very dilute aqueous acid. 

The following method is described in U.S. Patent 2,430,891. To a solution of 10 parts of tris-p-methoxyphenyl ethylene in 35 to 40 parts of carbon tetrachloride Is added a solution of 2.0 parts of chlorine in 50 parts of carbon tetrachloride, with stirring, and over a period of Vj hour. The carbon tetrachloride is then removed by distillation on a steam bath and the residual oil is recrystallized from 250 to 400 parts of methanol, decolorizing with charcoal or the like if necessary. Tris-p-methoxyphenyl chloroethylene is obtained in a yield of 65 to 75%. It melts at 113° to 114°C. 

Bromination. Neutral bromination of quinoline (66) using bromine in hot carbon tetrachloride and pyridine gave the 3-bromo derivative (68) (90%) and 3,6-dibromoquinoline (69) (2%), along with traces of 3,8-di-and 3,6,8-tri-bromo products [59CI(L) 1449 66AHC(7)1]. There is some... 

The use of the triphenylphosphine-carbon tetrachloride adduct for dehydration reactions appears to be a very simple way of synthesizing nitriles from amides, carbodi-imides from ureas, and isocyanides from monosubstituted formamides. All of these reactions involve the simultaneous addition of triphenylphosphine, carbon tetrachloride, and tri-ethylamine to the compound to be dehydrated. The elimination of the elements of water is stepwise. An adduct, e.g. (46), is first formed, chloroform being eliminated, which decomposes to produce hydrogen chloride and the dehydrated product. 

The reaction of aldehydes with carbon tetrachloride in the presence of excess tris(dimethylamino)phosphine has been used to prepare vinyl dihalides in yields of 50—70%. It is suggested that the reaction takes place via an intermediate salt (77), although the formation of this salt seems more likely to be analogous to the Perkow reaction than to involve attack on oxygen. 

The most critical decision to be made is the choice of the best solvent to facilitate extraction of the drug residue while minimizing interference. A review of available solubility, logP, and pK /pKb data for the marker residue can become an important first step in the selection of the best extraction solvents to try. A selected list of solvents from the literature methods include individual solvents (n-hexane, " dichloromethane, ethyl acetate, acetone, acetonitrile, methanol, and water ) mixtures of solvents (dichloromethane-methanol-acetic acid, isooctane-ethyl acetate, methanol-water, and acetonitrile-water ), and aqueous buffer solutions (phosphate and sodium sulfate ). Hexane is a very nonpolar solvent and could be chosen as an extraction solvent if the analyte is also very nonpolar. For example, Serrano et al used n-hexane to extract the very nonpolar polychlorinated biphenyls (PCBs) from fat, liver, and kidney of whale. One advantage of using n-hexane as an extraction solvent for fat tissue is that the fat itself will be completely dissolved, but this will necessitate an additional cleanup step to remove the substantial fat matrix. The choice of chlorinated hydrocarbons such as methylene chloride, chloroform, and carbon tetrachloride should be avoided owing to safety and environmental concerns with these solvents. Diethyl ether and ethyl acetate are other relatively nonpolar solvents that are appropriate for extraction of nonpolar analytes. Diethyl ether or ethyl acetate may also be combined with hexane (or other hydrocarbon solvent) to create an extraction solvent that has a polarity intermediate between the two solvents. For example, Gerhardt et a/. used a combination of isooctane and ethyl acetate for the extraction of several ionophores from various animal tissues. 

The most common reaction conditions for alkene reductions use excess tri-fluoroacetic acid and triethylsilane either neat202 204 or in an inert solvent such as nitrobenzene,134 2-nitropropane,205 carbon tetrachloride,206 chloroform,207 or dichloromethane.127,164 Reaction temperatures from —78° to well over 100° are reported. Ambient or ice-bath temperatures are most commonly used, but variations of these conditions abound. 

Lovelock and co-workers [228,229] determined methyl fluoride, methyl chloride, methyl bromide, methyl iodide, and carbon tetrachloride in the Atlantic Ocean. This shows a global distribution of these compounds. Murray and Riley [230,231] confirmed the presence of carbon tetrachloride, and also found low concentrations of chloroform and tri- and tetrachloroethylene in Atlantic surface waters. 

The selective activation of the primary hydroxyl group in methyl a-D-glucopyranoside by reaction with carbon tetrachloride and tris(dimethylamino)phosphine in A/.N-dimethylformamide at —40° has been reported.381 An alkoxytris(dimethylamino)phosphonium... 

In 1980, Gross and coworkers first applied this concept to a direct dehydrative glycosylation using tris(dimethylamino)phosphine and carbon tetrachloride [99]. 

Reversing this procedure will allow us to write a formula from a name. Let s try this with carbon tetrachloride and oxygen difluoride. The formulas for these two compounds are CCLt and OF2, respectively. 

Preparation of phosphorus trichloride. The following were placed in the flask F isopropyl alcohol (10 ml.), carbon tetrachloride (5 ml.) and glass wool. The taps between D and E and between G and H were opened, and G and D were cooled in liquid air. Radioactive phosphorus (1 g.) was placed in the vessel B, and non-radioaetive phosphorus trichloride (1 ml.) then added. B was then fixed in position and the bottom of the vessel heated so that the phosphorus tri-... 

The first isolable product in the reaction of triphenylphosphine and carbon tetrachloride is the salt (73), which reacts rapidly with further phosphine to give the stable phosphorane (74).62 In contrast, tris-t-butylphosphine reacts with germanium and tin tetrahalides to form the salts (75) 3 compounds of the latter type have long been postulated as arising from the reactions of phosphines with carbon tetrahalides but so far have defied detection. 

FIGURE 5. Proton NMR spectra of solutions prepared from (S)-a-phenylethylamine [(S)-22] (10 pL) (upper spectrum) and a mixture of (R)- and (S)-a-phenylethylamine (R)- and (S)-22] (7 and 5 J-L, respectively) (lower spectrum) in 0.3 mL of a carbon tetrachloride solution of tris[3-(ferf-butylhydroxymethylene)-(i-camphorato]europium(III) (96). The chemical shift scale applies only to the lower spectrum. Reprinted with permission from Reference 82. Copyright (1970) American Chemical Society... 

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