Toluene methods

If the toluene method to remove all the ethanol is not used, the yield is lower by 5-10%. 

Ethanol Toluene Method Ascending, one-dimensional development in a trough chamber with chamber saturation. 

Zinc foam (100 g) was shaken for 5 min with mercury(n) chloride (10 g), concentrated hydrochloric acid (5 ml), and water (150 ml), then the aqueous layer was poured off, and the amalgamated zinc was treated with water (75 ml), concentrated hydrochloric acid (175 ml), toluene (100 ml), and the carbonyl compound to be reduced (50 g). When necessary, glacial acetic acid (3-5 ml) may be added to increase the solubility in the aqueous layer. The mixture is heated to brisk ebullition under reflux. At each of three 6-hourly intervals hydrochloric acid (50 ml) is added, the total time of boiling being thus about 24 h. As examples, 3-oxo-3-phenyl-, -3-m-tolyl-, -3-p-tolyl-, -3-(l-naphthoyl)-, and -3-(2-naphthoyl)-propionic acid, benzoylnaphthalene, 2-acetylnaphthalene among other materials were reduced more satisfactorily than in absence of toluene. A comparison of the toluene method with the old method is provided, for instance, by Martin who obtained a 72-78 % yield in a preparation by himself by the old method, compared with 90% by the new method. 

The disulfide is obtained from the monosulfide with sulfur in boiling toluene (method A). The reaction is very slow but gives a high yield, and the disulfide is not contaminated with side products. The pure borane with mp 134-135° is isolated directly as a residue of concentrating the reaction mixture under vacuum or also by filtration the suspension. 

Thermal decomp, of acetylperoxide PR, radiometric toluene methods 338 kjk = 1680 60 Eva 1... 

The method of metallic mirrors was first to be used for the identification of radicals formed in the gas mixture (F. Paneth, 1929). Later the toluene method appeared (M. Szwarc, 1947) participation of radicals was concluded from the formation of... 

Without going into details of the chromatographic method, a SAR separation (asphaltenes having been eliminated) can be performed in a mixed column of silica followed by alumina. The saturated hydrocarbons are eluted by heptane, the aromatics by a 2 1 volume mixture of heptane and toluene, and the resins by a 1 1 1 mixture of dichloromethane, toluene and methanol. 

The water and sediment contents of crude oils is measured according to the standard methods NF M 07-020, ASTM D 96 and D 1796, which determine the volume of water and sediments separated from the crude by centrifuging in the presence of a solvent (toluene) and of a demulsifylng agent Table 8.13 gives the bottom sediment and water content of a few crude oils. 

The critical factor for any method involving an approximation or an extrapolation is its range of application. Liu et al. [15] demonstrated that the approach performed well for mutations involving the creation or deletion of single atoms. The method has also been successfully applied to the prediction of the relative binding affinities of benzene, toluene and o-, p-, and m-xylene to a mutant of T4-lysozyme [16]. In both cases, however, the perturbation to the system was small. To investigate range over which the extrapolation may... 

An alternative method of determining the completion of the reaction is to weigh the flask cmd toluene, emd to stop the passage of chlorine when the increase in weight is 37 g. 

Method 2. In a 500-ml. rovmd-bottomed flask, fitted with an efficient reflux condenser, place 92 g, (106 ml.) of toluene, 68 g. (41 ml.) of redistilled sulphuryl cldoride and 1 g, of dibenzoyl peroxide (Section IV,196). Reflux gently, when a vigorous reaction takes place the reaction is complete in 30 minutes. Isolate the benzyl chloride as described in Method 1. The yield is 50 g. 

Quantitative analysis. Spectroscopic analysis is widely used in the analysis of vitamin preparations, mixtures of hydrocarbons (e.y., benzene, toluene, ethylbenzene, xylenes) and other systems exhibiting characteristic electronic spectra. The extinction coefficient at 326 mp, after suitable treatment to remove other materials absorbing in this region, provides the best method for the estimation of the vitamin A content of fish oils. 

Characteristics of the system as nitrating reagents Wibaut, who introduced the competitive method for determining reactivities (his experiments with toluene, benzene and chlorobenzene were performed under heterogeneous conditions and were not successful), pointed out that solutions of nitric acid in acetic anhydride are useful in making comparisons of reactivities because aromatic compounds are soluble in them. ... 

Ingold and his co-workers used the competitive method in their experiments, in which nitration was brought about in acetic anhydride. Typically, the reaction solutions in these experiments contained o-8-I 4 mol of nitric acid, and the reaction time, depending on the reactivities of the compounds and the temperature, was 0-5-10 h. Results were obtained for the reactivities of toluene, > ethyl benzoate, the halogenobenzenes, ethyl phenyl acetate and benzyl chloride. Some of these and some later results are summarized in table 5.2. Results for the halogenobenzenes and nitrobiphenyls are discussed later ( 9.1.4, lo.i), and those for a series of benzylic compounds in 5,3.4. 

Although Pd is cheaper than Rh and Pt, it is still expensive. In Pd(0)- or Pd(ll)-catalyzed reactions, particularly in commercial processes, repeated use of Pd catalysts is required. When the products are low-boiling, they can be separated from the catalyst by distillation. The Wacker process for the production of acetaldehyde is an example. For less volatile products, there are several approaches to the economical uses of Pd catalysts. As one method, an alkyldi-phenylphosphine 9, in which the alkyl group is a polyethylene chain, is prepared as shown. The Pd complex of this phosphine has low solubility in some organic solvents such as toluene at room temperature, and is soluble at higher temperature[28]. Pd(0)-catalyzed reactions such as an allylation reaction of nucleophiles using this complex as a catalyst proceed smoothly at higher temperatures. After the reaction, the Pd complex precipitates and is recovered when the reaction mixture is cooled. 

All attempts to prepare selenazole derivatives by the Gatterman (for-mylation) or Friedel-Crafts (alkylation) methods failed (19, 26). indicating that the electrophilic reactivity of the 5-position is less than that of benzene or toluene. 

Specifications and Analytical Methods. Butanediol is specified as 99.5% minimum pure, determined by gas chromatography (gc), sohdifying at 19.6°C minimum. Moisture is 0.04% maximum, determined by Kad-Fischer analysis (dkecdy or of a toluene a2eotrope). The color is APHA 5 maximum, and the Hardy color (polyester test) is APHA 200 maximum. The carbonyl number is 0.5 mg KOH/g maximum the acetal content can also be measured dkecdy by gc. 

An alternative method consists of the reaction of trichloroacetonittile [545-06-2] with a hydrocarbon and AlCl. A ketimine is formed which is hydroly2ed by treatment with potassium hydroxide iato the nittile and chloroform. The reaction proceeds with aromatics such as toluene and phenols (130). 

Ammonium lactate [34302-65-3] ia coaceatrated aqueous solutioas has beea coaverted to ammonia and the ester by alcoholysis at temperatures ranging from 100—200°C usiag a variety of alcohols and water entrainers, such as toluene. Ester yields ranging from 50—80% were obtained. This method has also been suggested as a recovery and purification method from impure solutions of lactate (29). However, a considerable amount of the lactate is not converted to the recoverable ester and is lost as lactamide (6). 

Attempts have been made to develop methods for the production of aromatic isocyanates without the use of phosgene. None of these processes is currently in commercial use. Processes based on the reaction of carbon monoxide with aromatic nitro compounds have been examined extensively (23,27,76). The reductive carbonylation of 2,4-dinitrotoluene [121 -14-2] to toluene 2,4-diaLkylcarbamates is reported to occur in high yield at reaction temperatures of 140—180°C under 6900 kPa (1000 psi) of carbon monoxide. The resultant carbamate product distribution is noted to be a strong function of the alcohol used. Mitsui-Toatsu and Arco have disclosed a two-step reductive carbonylation process based on a cost effective selenium catalyst (22,23). 

A convenient method for the synthesis of these low boiling materials consists of the reaction of /V,/V-dimethy1iirea [96-31-1] with toluene diisocyanate to yield an aUphatic—aromatic urea (84). Alternatively, an appropriate aUphatic—aromatic urea can be prepared by the reaction of diphenylcarbamoyl chloride [83-01-2] with methylamine. Thermolysis of either of the mixed ureas produces methyl isocyanate ia high yield (3,85). 

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