From carbon tetrachloride and

A similar reaction of 1,5-cyclooctadiene with trichloromethyl radicals, produced from carbon tetrachloride and dibenzoyl peroxide, leads to 2-chloro-6-trichloromethylbicyclo-[3.3.0]octane (94), with chloroform and dibenzoyl peroxide the analogue 95 is obtained and iV-t-butylfonnamide affords compound 96 (equation 57)62,63. 

The tertiary amine thus obtained was dissolved in absolute ethanol and was refluxed for two days with five molar percent excess of the appropriate bromoalkane (97% Humphrey Chemical, North Haven, Conn.). Solvent was removed and the residue in aqueous Na2C03 solution was extracted with hexane to remove any unreacted bromoalkane. Next, the N-alkyl N-benzyl N-methylglycine was extracted into chloroform from the aqueous layer. Solvent was stripped off and the crude material was recrystallized thrice from carbon tetrachloride and twice from THF/CHCl3 (60 40 v/v) mixture. The yields of the purified betaines were about 75% of the theoretical. 

Carbon ditelluride has not yet been prepared. Attempts to prepare this compound from carbon tetrachloride and hydrogen telluride, carbon tetrabromide or tetraiodide and silver telluride, carbon and tellurium2, or dichloromethane and tellurium3 were unsuccessful. The claim of the preparation of carbon ditelluride by sputtering tellurium from a tellurium/graphite electrode in a DC-arc under carbon disulfide4 was withdrawn5. 

Colour Test. Tetrachloroethylene may be distinguished from carbon tetrachloride and chloroform by the following test to 5 ml in a stoppered cylinder add 5 ml of bromine solution and shake vigorously at intervals of 15 minutes for 1 hour—bromine colour fades and there is a white turbidity in the lower layer. 

In Italy and France phosgene was prepared during the first years of the war of 1914-18 from carbon tetrachloride and fuming sulphuric acid according to the method of Schiittzenberger modified by Grignard. ... 

During the war large quantities were obtained as a by-product in the preparation of phosgene from carbon tetrachloride and oleum (see p. 61). 

Standard cardiorespiratory resuscitation and antiarrhythmia treatment are used for acute solvent poisoning. Toxicity from carbon tetrachloride and chloroform involves the generation of phosgene (a 1914-18 war gas) which is inactivated by cysteine, and by glutathione which is formed from cysteine treatment with N-acetylcysteine, as for poisoning with paracetamol, is therefore recommended. 

Free radicals from certain halogenated xenobiotics Incorporate Into phospholipid. Trudell et al. (81,82) have shown that free radicals from carbon tetrachloride and halothane add to the double bonds of fatty acyl chains of phospholipids In the membrane surrounding cytochrome P-450. Oleic acid moieties were converted... 

Although free trifluoromethyl cation salts have not yet been isolated and characterized, it is possible to generate a mixture of chlorofluoromethyl cations (CFyClj., ) in situ from carbon tetrachloride and strong Lewis acids [8]. These systems can be used for electrophilic trihalomethylation of electron-rich aromatic substrates. The remaining chlorine substituents are substituted by fluorine with 70% HF-pyridine (Scheme 2.141). 

N-Maleimido)bemyldimethylamine (/F). Cyclization of (III) to (IV) is as follows To 0.5 g (2 mmoles) of (III) and 90 mg of anhydrous sodium acetate is added 1 ml of acetic anhydride, and the pastry mixture is stirred at 100° for about 5 min until a deep yellow solution forms. This is added to 60 ml of cold water. The mixture is extracted twice with 25 ml of methylene chloride, and the extracts are discarded. The mixture is adjusted to pH 7.0-7.5 with about 30 ml of 1 Jlf NaHCOs and extracted three times with 25 ml of methylene chloride. These extracts are combined, dried over MgSOi, and filtered, and the solvent is removed. The product is recrystallized from carbon tetrachloride and hexane to give bright yellow crystals of m.p. 86°-87° in about 80% yield. Compound (IV) polymerizes readily however, the polymer is insoluble in carbon tetrachloride and can be removed by filtration. 

Aminoazobenzene is freely soluble in methylated spirit, although insoluble in water. For recrystallisation, therefore, dissolve the crude substance in boiling methylated spirit, remove from the water-bath, and then add water drop by drop until the solution becomes just cloudy owing to the separation of the solute replace the solution momentarily on the water-bath until the cloudiness disappears, and then at once remove the solution, and allow it to cool slowly. (Alternatively, the crude dry material can be reciystallised from carbon tetrachloride in the usual way.) Aminoazobenzene is thus obtained as yellowish-brown crystals, m.p. 126° yield, 5 g. 

Method 2. Place 0-2 g. of cupric acetate, 10 g. of ammonium nitrate, 21 2 g. of benzoin and 70 ml. of an 80 per cent, by volume acetic acid -water solution in a 250 ml. flask fitted with a reflux condenser. Heat the mixture with occasional shaking (1). When solution occurs, a vigorous evolution of nitrogen is observed. Reflux for 90 minutes, cool the solution, seed the solution with a crystal of benzil (2), and allow to stand for 1 hour. Filter at the pump and keep the mother liquor (3) wash well with water and dry (preferably in an oven at 60°). The resulting benzil has m.p. 94-95° and the m.p. is unaffected by recrystallisation from alcohol or from carbon tetrachloride (2 ml. per gram). Dilution of the mother liquor with the aqueous washings gives a further 1 Og. of benzil (4). 

To prepare triphenylcarbinol from triphenylchloromethane, boil the latter with excess of water for 10 minutes. Filter off the resulting triphenylcarbinol, dry between filter papers, and recrystallise from carbon tetrachloride or alcohol m.p. 162°. The yield is almost quantitative. 

Method 2. Place 90 g. of sodium benzenesulphonate (Section IV,29) (previously dried at 130-140° for 3 hours) and 50 g. of powdered phosphorus pentachloride (1) in a 500 ml. round-bottomed flask furnished with a reflux condenser heat the mixture in an oil bath at 170-180° for 12-15 hours. Every 3 hours remove the flask from the oil bath, allow to cool for 15-20 minutes, stopper and shake thoroughly until the mass becomes pasty. At the end of the heating period, allow the reaction mixture to cool. Pour on to 1 kilo of crushed ice. Extract the crude benzenesulphonyl chloride with 150 ml. of carbon tetrachloride and the aqueous layer with 75 ml. of the same solvent. Remove the solvent under atmospheric pressure and proceed as in Method 1. The yield is about 170 g., but depends upon the purity of the original sodium benzenesulphonate. 

Azlactone of a-acetylaminocinnamic acid. Warm a mixture of 29 g. of acetylglycine, 39-5 g. (37 -5 ml.) of redistilled benzaldehyde (Section IV,115), 15 g. of anhydrous sodium acetate and 67 g. (62 ml.) of acetic anhydride (95 per cent.) in a 500 ml. conical flask (equipped with a reflux condenser) on a water bath with occasional stirring until solution is complete (10-20 minutes). Boil the resulting solution for 1 hour, cool and leave in a refrigerator overnight. Stir the sohd mass of yellow crystals with 60 ml. of cold water, transfer to a Buchner funnel and wash well with cold water. (If the odour of benzaldehyde is stih apparent, wash with a little ether.) Recrystallise from carbon tetrachloride or from ethyl acetate-hght petroleum. The yield of azlactone, m.p. 150°, is 35 g. 

Triiodobenzoyl chloride. Reflux 5 g. of 3 4 5-triiodo-benzoic acid, m.p. 289-290°, gently with 10 ml. of redistilled thionyl chloride for 2 hours. Distil off the excess of thionyl chloride on a water bath, and recrystallise the residue from carbon tetrachloride - light petroleum with the use of a little decolourising charcoal. The yield of the acid chloride (bright yellow needles, m.p. 138°) is 3-8 g. it keeps well in a stoppered bottle. 

Place a mixture of 30 g. of 3 5-dinitrobenzoic acid (Section IV,168 and 33 g. of phosphorus pentachloride in a Claisen flask fit a reflux condenser into the short neck and cork the other neck and side arm (compare Fig. Ill, 31, 1). Heat the mixture in an oil bath at 120-130° for 75 minutes. Allow to cool. Remove the phosphorus oxychloride by distillation under reduced pressure (25°/20 mm.) raise the temperature of the bath to 110°. The residual 3 5-dinitrobenzoyl chloride solidifies on cooling to a brown mass the yield is quantitative. Recrystallise from carbon tetrachloride the yield is 25 g., m.p. 67-68° and this is satisfactory for most purposes. Further recrystallisation from a large volume of light petroleum b.p. 40-60°, gives a perfectly pure product, m.p. 69 -6°. 

The longer perfluoroalkanesulfonic acids are hydroscopic oily Hquids. Distillation of the acid from a mixture of its salt and sulfuric acid gives a hydrated mixture with melting points above 100°C. These acids show the same general solubiUties as trifluoromethanesulfonic acid, but are insoluble in ben2ene, heptane, carbon tetrachloride, and perfluorinated Hquids. AH of the higher perfluoroalkanesulfonic acids have been prepared by electrochemical fluorination (20). 

Confirmation of the destmetion of ozone by chlorine and bromine from halofluorocarbons has led to international efforts to reduce emissions of ozone-destroying CPCs and Halons into the atmosphere. The 1987 Montreal Protocol on Substances That Deplete the Ozone Layer (150) (and its 1990 and 1992 revisions) calls for an end to the production of Halons in 1994 and CPCs, carbon tetrachloride, and methylchloroform byjanuary 1, 1996. In 1993, worldwide production of CPCs was reduced to 50% of 1986 levels of 1.13 x 10 and decreases in growth rates of CPC-11 and CPC-12 have been observed (151). 

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