Carbon tetrachloride solution

The mono-bromination of phenol at low temperatures in carbon disulphide or carbon tetrachloride solution results in almost exclusive para substitution ... 

The use of ether may be avoided by mixing the ester, after its isolation from the water layer, with about 20 ml. of carbon tetrachloride. The carbon tetrachloride solution then forms the lower layer in all washing operations (compare Methyl Benzoate, Section IV,176). 

Unlike nitration. 2-amino-4-methylselenazole can be directly bromi-nated, using bromine in carbon tetrachloride solution, to give 2-amino-5-bromo-4-methylselenazole hydrobromide [m.p. 180°C (decomp.)] (19). The free base cannot be isolated. Use of excess of bromine can lead to destruction of the molecule. 

Bulk polymerization has been studied at relatively low temperatures and in toluene and carbon tetrachloride solutions carried to low conversions (12). The effects of temperature and different organic peroxide initiators have been observed. The molecular weight of soluble polymer after 3% conversion is ca — 19,000 and is somewhat dependent on initiator concentration or temperature between 35 and 65 °C. With di-2-methylpentanoyl... 

The nmr spectmm of PVAc iu carbon tetrachloride solution at 110°C shows absorptions at 4.86 5 (pentad) of the methine proton 1.78 5 (triad) of the methylene group and 1.98 5, 1.96 5, and 1.94 5, which are the resonances of the acetate methyls iu isotactic, heterotactic, and syndiotactic triads, respectively. Poly(vinyl acetate) produced by normal free-radical polymerization is completely atactic and noncrystalline. The nmr spectra of ethylene vinyl acetate copolymers have also been obtained (33). The ir spectra of the copolymers of vinyl acetate differ from that of the homopolymer depending on the identity of the comonomers and their proportion. 

These values assume chlorination in carbon tetrachloride solution under homogeneous conditions favoring random distribution of chlorine atoms along the chain. Viscous reaction conditions, faster chlorine addition rates, lower temperature conditions, etc, can lead to higher AH at equivalent chlorine levels because of more blocky chlorine distribution on the polymer chain. 

A radical reaction is sometimes observed to compete with the particularly slow acid hydrolyses of diaziridines derived from formaldehyde. With other diaziridines the radical reaction can be made to predominate by using HCl in carbon tetrachloride solution. Acetaldehyde, butyraldehyde, butylamine and ammonia are obtained from (160) (64CB49). 

These formulae explain the scission products of the two alkaloids and the conversion of evodiamine into rutaecarpine, and were accepted by Asahina. A partial synthesis of rutaecarpine was effected by Asahina, Irie and Ohta, who prepared the o-nitrobenzoyl derivative of 3-)3-amino-ethylindole-2-carboxylic acid, and reduced this to the corresponding amine (partial formula I), which on warming with phosphorus oxychloride in carbon tetrachloride solution furnished rutaecarpine. This synthesis was completed in 1928 by the same authors by the preparation of 3-)S-amino-ethylindole-2-carboxylic acid by the action of alcoholic potassium hydroxide on 2-keto-2 3 4 5-tetrahydro-3-carboline. An equally simple synthesis was effected almost simultaneously by Asahina, Manske and Robinson, who condensed methyl anthranilate with 2-keto-2 3 4 5-tetrahydro-3-carboline (for notation, see p. 492) by the use of phosphorus trichloride (see partial formulae II). Ohta has also synthesised rutaecarpine by heating a mixture of 2-keto-2 3 4 5-tetrahydrocarboline with isatoic anhydride at 195° for 20 minutes. 

A systematic investigation of compounds of these types by Mason has recently placed this subject on a firm basis. The infrared spectra of chloroform and carbon tetrachloride solutions of... 

A l-Iiter, three-necked, round-bottom flask is equipped with a mechanical stirrer, a thermometer immersed in the reaction mixture, a dropping funnel, and a gas vent. In the flask is placed a mixture of 96% sulfuric acid (25.5 ml, 470 g, 4.8 mole), carbon tetrachloride (100 ml), and adamantane (13.6 g, 0.10 mole), and the mixture is cooled to 15-20° with rapid stirring in an ice bath. One milliliter of 98% formic acid is added and the mixture is stirred until the evolution of carbon monoxide is rapid (about 5 minutes). A solution of 29.6 g (38 ml, 0.40 mole) of t-butyl alcohol in 55 g (1.2 mole) of 98-100% formic acid is then added dropwise to the stirred mixture over 1-2 hours, the temperature being maintained at 15-20°. After stirring for an additional 30 minutes, the mixture is poured onto 700 g of ice, the layers are separated, and the aqueous (upper) layer is extracted three times with lOO-ml portions of carbon tetrachloride. The combined carbon tetrachloride solutions are shaken with 110 ml of 15 A ammonium hydroxide, whereupon ammonium 1-adamantanecarboxylate forms as a crystalline solid. This precipitate is collected by filtration through a fritted glass funnel and washed... 

A 100-ml flask is charged with 25 ml of bromine and 10 g of adamantane and heated under reflux for 3 hours. The cooled mixture is dissolved in 100 ml of carbon tetrachloride, and the carbon tetrachloride solution is washed with 100-ml portions of saturated bisulfite solution until the color of bromine is discharged. The solution is then washed twice with water and dried (magnesium sulfate). The solvent is removed (rotary evaporator) and the product is recrystallized from methanol. (For best recovery of the recrystallized material, the methanol solution should be cooled in a Dry Ice cooling bath.) The product has mp 108°. 

On treatment with bromine in carbon tetrachloride solution, it yields a dibromide in which two atoms of bromine have been fixed in the pro-penyl side chain, melting at 85° to 86°. 

C. 2-Phenylethyl benzoate. The carbon tetrachloride solution of N-nitroso-N-(2-phenylethyl)benzamide (Note 4) and 0.1 g. of sodium carbonate (Note 5) are placed in a 200-mi. round-bottomed flask equipped with a condenser, and the mixture is heated under reflux for 24 hours. The evolution of nitrogen ceases, and the yellow color of the nitrosoamide disappears near the end of this period. The solution is washed with 5% sodium hydroxide solution, water, and dried. The solvent is removed under reduced pressure and the 2-phenylethyl benzoate distilled b.p. 138-142° (1 mm.), yield 5.8-6.1 g. [56-59% based on N-(2-phenylethyl) benzamide]. 

B. Wet process Discussion. The sulphide is oxidised (1) by bromine in carbon tetrachloride solution, followed by nitric acid, (2) by sodium chlorate and hydrochloric acid, or (3) by a mixture of nitric and hydrochloric acids and a little bromine. The use of the first-named oxidising agent will be described the reaction may be represented by ... 

Oxa-4,5-benzotricyclo[4.1.0.02-7]heptene was readily converted to 1-benzoxepin (1) on treatment with silver(I) perchlorate. Dicarbonylrhodium chloride dimer or j3-allylpalladium chloride dimer can also be used as catalyst. Thermolysis of the starting material in carbon tetrachloride solution gives 2a,7b-dihydrocyclobuta[6]benzofuran (2) as a new isomer. Depending on the temperature the proportion of 2 varies from 50% (150°C) to 100% (225°C).110... 

Dimethyl 4-ethoxy-2,7-dimethyl-4,5-dihydro-l 7/-azepine-3,6-dicarboxylate (1) with sodium ethoxide in refluxing diethyl ether, or on standing at room temperature in carbon tetrachloride solution, readily loses ethanol to yield dimethyl 2,7-dimethyl-4//-azepine-3,6-dicar-boxylate (2).29 The 4-methoxy derivative is also unstable and on warming at 100 C under reduced pressure loses methanol to yield the same product (44%).120... 

In the related paper on 19F screening parameters of para-substituted fluorobenzenes in relation to resonance effects, a few measurements for SOMe and S02Me were recorded but no use was made of them for calculation of years later, Sheppard and Taft113 used these data (carbon tetrachloride solution) to calculate nR values through equation 11 ... 

Braverman and Reisman111 have found that addition of a carbon tetrachloride solution of bromine to bis-y,y-dimethylallenyl sulfone 20 at room temperature unexpectedly resulted in spontaneous and quantitative fragmentation of the sulfone, with formation of the cyclic a, /3-unsaturated sulfmate (y-sultine) 43a and the tribromo products 44 and 45 (equation 38). Analogously, treatment of the same sulfone with trifluoroacetic acid gives rise to y-sultine 43b. It is interesting to note that from a synthetic point of view it is not even necessary to prepare the diallenyl sulfone 20, since one can use its sulfinate precursor (equation 24) to obtain exactly the same results, under the same conditions. The authors suggested that the fragmentation-cyclization of sulfone 20 may take place by the mechanism depicted in equation 39. 

In a dry, 1-1., two-necked flask, equipped with a mechanical stirrer and a reflux condenser fitted with a drying tube, are placed 17.8 g. (0.100 mole) of anthracene (Note 1), 27.2 g. (0.202 mole) of anhydrous cupric chloride (Note 2), and 500 ml. of carbon tetrachloride (Note 3). The reaction mixture is stirred and heated under reflux for 18-24 hours. The brown cupric chloride is gradually converted to white cuprous chloride, and hydrogen chloride is gradually evolved. At the end of the reaction the cuprous chloride is removed by filtration, and the carbon tetrachloride solution is passed through a 35-mm. chromatographic column filled with 200 g. of alumina (Note 4). The column is eluted with 400 ml. of carbon tetrachloride. The combined eluates are evaporated to dryness to give 19-21 g. (89-99%) of 9-chloroanthracene as a lemon-yellow solid, m.p. 102-104° (Note 5). Crystallization of the product from petroleum ether... 

The decolonization of the yellow product (Note 11) is achieved by dissolving the product in an equal volume of carbon tetrachloride (ca. 12 ml.) and vigorously shaking the solution thus obtained with 1.5 ml. of a freshly prepared aqueous 35% sodium thiosulfate. The two layers are completely separated after 5 minutes. The colorless bottom layer is drawn off into a 50-ml. Erlenmeyer flask. The top layer is extracted three times with 1.5 ml. of carbon tetrachloride. The combined carbon tetrachloride solution is dried over 0.5 g. (Note 12) of anhydrous magnesium sulfate for 30 minutes. The solution is then filtered into a 50-ml. distilling flask, and the magnesium sulfate is washed several times with carbon tetrachloride (total 5 ml.). The solvent is removed, and the colorless product is distilled as described above, affording 14.7-15.8 g. (69-74% overall, based on hexanoic acid 88-92% for the decolonization step) of colorless 2-bromohexanoyl chloride, b.p. 45-47° (1.5 mm.), n22 d 1.4706 (Note 13), i 4 1.4017 (Notes 14 and 15). 

Fluid Liquid Tap water, Dist. water. De-ion. water, R-134a, Methanol, Isopropanol, Carbon tetrachloride solutions with several ionic compositions... 

A singlet precursor has, however, been proposed for 4,4,4-triohloro-2-methyl-1-butene (17) produced in the photolysis of isomesityl oxide (18) in carbon tetrachloride solution on the basis of its all-emission spectrum (DoMinh, 1971). There remains some ambiguity, however, about the detailed route by which 17 is formed. Moreover there is other evidence suggesting that ketone photolysis in carbon tetrachloride is different CI3C. CHaCiMe) CHa CH3. CO. CHa. C(Me) CHa... 

The exocyclic a,P-unsaturated ketones la-h used for the preparation of dibromides 2a-h were E isomers synthesized by known procedures (refs. 7,8). Previously we reported the synthesis of some dibromides (2a,d,g) used here as starting materials, by the bromine addition of the appropriate a,P-unsaturated ketones (la,d,g) (ref. 6). In the case of our present study, compounds lb,c,e,f,h were allowed to react with a small excess of bromine in carbon tetrachloride solution at room temperature for approx. 20 min. to afford the dibromides 2b,c,e,f,h (Eqn. 1) (Table 1). 

Eor plant and soil samples, transfer the carbon tetrachloride solution into a glass column packed with 7g of silica gel samrated in carbon tetrachloride. Rinse... 

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