Separation, of primary, secondary and

Hinsberg procedure for the separation of primary, secondary and tertiary amines is given under (viii) above, and this method may be used. The following experimental details may, however, be found useful for the preparation of derivatives of primary and secondary amines. 

The separation of primary, secondary and tertiary amines using toluene-p-sulphonyl chloride (Hinsberg s method) is described in Section 9.7. 

Arylsulfonyl chlorides react with primary and secondary amines with the formation of sulfonamides, which are used both for the separation of primary, secondary, and tertiary amines, and for the identification of the former two types of compounds. For identification benzenesulfonyl chloride (80, 81) and p-toluenesulfonyl chloride (82) are especially suitable. 

Hofmann amine separation org chem A technique to separate a mixture of primary, secondary, and tertiary amines they are heated with ethyl oxalate there is no reaction with tertiary amines, primary amines form a diamide, and the secondary amines form a monoamide when the reaction mixture is distilled, the mixture is separated into components. haf-mon am,en, sep-3,ra-sh3n ... 

The nitrosamines are neutral oily liquids of little importance in themselves. This reaction, however, serves to separate secondary bases from mixtures of primary, secondary and tertiary. The aromatic nitrosamines undergo an interesting rearrangement when heated with alcoholic hydrochloric acid (B., 20, 1247), the nitroso group migrating to a position in the nucleus, forming p-nitroso compounds. 

Mixtures of primary, secondary and tertiary amines can usually be separated by Hinsberg s method. This is based on the fact that reaction with benzene-sulphonyl (or toluene-p-sulphonyl) chloride converts primary amines into alkali-soluble sulphonamides, secondary amines into alkali-insoluble sulphon-amides and leaves tertiary amines unaffected. 

This article surveys the research work on the synthesis and modification reactions of poly(ethyleneimine) as well as its applications to metal complexation processes. Poly-(ethyleneimine), one of the most simple heterochain polymers exists in the form of two different chemical structures one of them is branched, which is a commercially available and the other one linear which is synthesized by cationic polymerization of oxazoline monomers and subsequent hydrolysis of polyf(/V acylimino)cthylcne]. The most salient feature of poly(ethyleneimine) is the simultaneous presence of primary, secondary, and tertiary amino groups in the polymer chain which explains its basic properties and gives access to various modification reactions. A great number of synthetic routes to branched and linear poly(ethyleneimine)s and polymer-analogous reactions are described. In addition, the complexation of polyfethyleneimine) and its derivatives with metal ions is investigated. Homogeneous and heterogeneous metal separation and enrichment processes are reviewed. 

The reaction of ammonia with primary alkyl halides generally forms a mixture of primary, secondary, and tertiary amines and even a certain amount of the quaternary ammonium halide. Still, the method may be profitable for obtaining primary amines if the halogen compound is above C, and excess ammonia is employed, for then polyalkylation is less likely and the products, having widely different boiling points, are more readily separated. Thus w-butyl bromide and a large excess of ammonia in alcohol solution at room temperature give a 47% yield of w-butylamine. ... 

The substitution reaction by ammonia and other amines can give rise to complex mixtures of primary, secondary and tertiary amines, together with quaternary ammonium salts (see Scheme 2.4). The separation of these by chemical means, as opposed to distillation or chromatography, is discussed in the section on amines. 

A laboratory reactor system was constructed for the investigation of tar conversion under real fixed-bed conditions. The basic idea behind the reactor design was the spatial separation of primary pyrolysis and secondary tar reactions. A scheme of the system is shown in fig, 2. After the primary pyrolysis stage, the tar containing pyrolysis gas is swept to the conversion reactors where homogeneous and/or heterogeneous tar reactions can be investigated. 

F) Separation of Amines by the Use of Benzenesulfonyl Chloride (Hinsbei Reaction). For this experiment the primary, secondary, and tertiary butylamines may be used, or aniline, methyl-aniline and dimethylaniline. To 1 ml of primary, secondary, and tertiary amine, in separate tubes, add 5 ml of 6 A sodium hydroxide solution, 4 ml of water, and 2 ml of benzenesulfonyl chloride. The tubes are stoppered and shaken at intervals for 5 minutes while they are warmed in a water bath. The rate at which heat is... 

Conductivity detection in both of its modes of application is also suitable for the detection of primary, secondary, and tertiary alkylamines. This is shown in Fig. 3-139 using three methylamines which are separated on Vydac 400 IC 405 with isonicotinic acid as the eluent. Interferences are possible if the sample contains potassium, rubidium, and/or cesium in addition to amines. However, a small variation of the solvent content in the mobile phase which mainly affects the retention of alkylsubstituted cations, allows the optimization of the separation. In comparison to Fig. 3-140, the separation of the... 

The alkyl amines as prepared are usually in the form of their hydrochlorides or other hydrohalides, and consist of a mixture of primary, secondary and tertiary amines... I have disclosed methods (see below) by which the primary, secondary and tertiary amines may be separated from each other. 

The high-temperature thiation of thiophosgene with elemental sulfur leads to a multitude of primary, secondary, and tertiary reaction products <2000SUL23> the product mixture was separated and assigned by gas chromato-graphy-mass spectrometry (GC-MS), including the unequivocal identification of 2,2, 4,4, 6,6 -hexachloro-l,3,5-trithiane. 

If alkyl halides are heated with phosphonium iodide in the presence of zinc oxide at 100-180 C, progressive alkylation takes place and the mixture of primary, secondary and tertiary phosphines can be separated by fractional distillation (6.29, 6.30). In the absence of zinc oxide, tertiary phosphines and quaternary phosphonium compounds are the favoured products (6.31,6.38). 

It is now clear why the relative strengths in water are not adequate to account for the catalytic effects of primary, secondary, and tertiary amines in non-aqueous solvents, since the effect of hydration will not operate in the latter case. The position is similar even when both rates and equilibria are studied in aqueous solution, since the transfer of the proton is incomplete in the transition state, and the interaction with the solvent will be less than it is in the final state, in which the proton has been completely transferred. This picture agrees with the observation that in the plots of Ig/Cb against pK(H20) in the decomposition of nitramide the separation between primary and tertiary amines is much greater for k a.niso Q) than for /Cb(H20). 

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