Toluene, extraction with

Sediments NF M 07-010 ISO 3735 ASTM D 473 Extraction with toluene and weighing of residue... 

A mixture of 2-chloro-A-(2-hydroxyl-l-methyl-2-phenylethyl)benzamide (44) (9.5g, 24.9 mmol) and P2O5 in o-chlorobenzene (1,50 mL) was refluxed overnight. Upon completion, the reaction was cooled to room temperature and then chilled to 0 °C. To the crude reaction mixture, 300 mL of water was cautiously added. The resulting dark solution was washed with toluene (2 x 50 mL). The aqueous layer was cooled to 0 °C and 50% NaOH added to final pH of 11. The resulting mixture was extracted with toluene (4 x 50 mL). The toluene fractions were combined, dried, filtered and concentrated in vacuo. The residue was crystallized from benzene to afford l-(2-chlorophenyl)-3-methylisoquinoline (45) as a white solid (6.68g, 80%). M.P. = 107-108 °C H NMR (CDCI3) S 8.45 (s, IH), 8.11 (d, IH), 7.85 (dt, IH), 7.41-7.68 (bm, 6H), 2.51 (s, 3H). 

The free base, N,N -4,10<)ioxa-3,11 <)ioxotridecvlene-1,13-bis-tetrahydropapaverine, was obtained by basifying an aqueous solution of the dioxalate with sodium bicarbonate solution, followed by extraction with toluene and evaporation of the solvent, to give a colorless viscous oil. 

To a solution of 35.3 parts of phenylacetonitrile and 47.6 parts of 2-bromopyridine in 175 parts of dry toluene is added 53.4 parts of sodamide slowly with stirring over a period of 45 minutes. The resultant mixture is stirred at 100 C for 2 hours before it is cooled and the excess sodamide is decomposed by the addition of water. The toluene layer is separated and washed with water to remove excess alkali. The toluene solution is extracted with 6N hydrochloric acid and the acid extract is made alkaline and then extracted with toluene. The toluene solution is dried over sodium sulfate and the solvent is evaporated. Recrystal-lization of the residue from alcohol-hexane gives a-phenvl-2-pyridineacetonitrile melting at about 87°-88°C. 

The toluene layer is separated and washed with water and extracted with 6N hydrochloric acid. The acid extract Is made alkaline and extracted with toluene. The toluene solution is washed with water and dried and the solvent is evaporated. Distillation of the residue gives 4-diisopropvlamino-2-phenvl-2-(2-pvridyl)-butvronitrile boiling at about 145 -160°C at 0.3 mm pressure. 

To a stirred and refluxed suspension of 17 parts of 1,2-dibromoethane, 7.8 parts of sodium hydrogen carbonate and 50 parts of 2-propanol is added a mixture of 3.4 parts of dl-2-thio-1-phenyl-lmidazolidine, 9 parts of a 20% potassium hydroxide solution in 40 parts of 2-propanol over a period of about 1 hour. After the addition is complete, the whole is stirred and refluxed for an additional 3 hours. The reaction mixture is evaporated. To the residue are added 18 parts of a 15% potassium hydroxide solution. The whole is extracted with toluene. The extract is dried and evaporated. The oily residue is dissolved in acetone and gaseous hy-... 

This reaction mixture is kept between 0°C and -i-5°C for six hours, with agitation and under an inert atmosphere, then 5 cc of a 0.2N solution of acetic acid in toluene are added. The mixture is extracted with toluene, and the extracts are washed with water and evaporated to dryness. The residue is taken up in ethyl acetate, and then the solution Is evaporated to dryness in vacuo, yielding a resin which is dissolved in methylene chloride, and the solution passed through a column of 40 g of magnesium silicate. Elution is carried out first with methylene chloride, then with methylene chloride containing 0.5% of acetone, and 0.361 g Is thus recovered of a crude product, which is dissolved in 1.5 cc of isopropyl ether then hot methanol Is added and the mixture left at 0°C for one night. 

Davis and co-workers have carried out the first examples of the Knoevenagel condensation and Robinson annulation reactions [61] in the ionic liquid [HMIM][PFg] (HMIM = l-hexyl-3-methylimidazolium) (Scheme 5.1-33). The Knoevenagel condensation involved the treatment of propane-1,3-dinitrile with a base (glycine) to generate an anion. This anion added to benzaldehyde and, after loss of a water molecule, gave l,l-dicyano-2-phenylethene. The product was separated from the ionic liquid by extraction with toluene. 

The Robinson annulation of ethyl acetoacetate and trans-chalcone proceeded smoothly to give 6-ethoxycarbonyl-3,5-diphenyl-2-cyclohexenone in 48 % yield. The product was separated from the ionic liquid by solvent extraction with toluene. In both these reactions, the ionic liquid [HMIM][PF6] was recycled and reused with no reduction in the product yield. 

A mixture of the thiosalicylamide 1 (32.0 g, 120 mmol), TsOH (1.0 g, 6 mmol) and toluene (1.5L) was heated under reflux for 15 h while a mixture of EtOH and toluene (30 mL) was allowed to distill off. The cooled reaction mixture was washed with sat. aq NaHC03 (60 mL), the aqueous layer was extracted with toluene (2 x 30 mL) and the organic phases were combined, dried and evaporated. Sublimation of the residue in vacuo gave the yellow product yield 16.6 g (77%) mp 143.5-145rC (ligroin). 

Fish Grinding of sample and extraction with toluene clean-up extract on alumina column GC/ECD 0.005 pg/L ( "endo-sulfan) 0.005 pg/L ( "endosulfan) 0.025 pg/L (endosulfan sulfate) 84 ( "endosulfan) 79 ( "endosulfan) 86 (endosulfan sulfate) Zoun et al. 1987... 

Samples for determination of ionic alky Head species in marine fauna were homogenized in the presence of salts and the alkyllead component was extracted with toluene and oxidized with HN03. Determination was by DPASV115. A method based on oxidation on Hg electrode has been described116 for analysis of alkylleads in gasoline. Alkylation of Hg is involved, of course, but as an oxidation the method does not suffer from the background of atmospheric oxygen. The peak potentials Ev for oxidation of tetramethyllead and tetraethyllead on various cathodes are well resolved (Table 5). 

Synthesis of 8,8-Bis(cyclopentadienyl)-7,9-bis(trimethylstannyl)-8-zirconabicyclo[4.3.0]nona-1 (9),6(7)-diene 109 (Scheme 7.31) [172] To a solution of bis(cyclopentadienyl)zirconium dichloride (585 mg, 2.0 mmol) in THF (10 mL) at — 78 °C was added dropwise a solution of w-butyllithium in hexane (2.4 mL, 4.0 mmol). After the reaction mixture had been stirred at — 78 °C for 1 h, a solution of l,8-bis(trimethylstannyl)-l,7-octadiyne (863 mg, 2.0 mmol) in THF (2 mL) was added at the same temperature. The temperature was then allowed to rise to ambient, and the mixture was stirred for a further 3 h. The solvent was then removed under reduced pressure and the product was extracted with toluene. The extracts were filtered and the filtrate was concentrated and kept at 0°C to afford the product 109 (723 mg, 55% yield). 

Bartlett et al. [55] used the method of Uthe et al. [70] for determining methylmercury. Sediment samples of 2-5g were extracted with toluene after treatment with copper sulphate and an acidic solution of potassium bromide. Methylmercury was then back extracted into aqueous sodium thiosulphate. This was then treated with acidic potassium bromide and copper sulphate following which the methylmercury was extracted into pesticide grade... 

Theory Selenium is very toxic and its contamination is usually controlled by an absorptiometric method after destruction of the organic compound with fuming nitric acid. The latter converts selenium (Se) as selenous acid (H2Se03), which on subsequent treatment with 3,3 -diaminobenzidinc under controlled experimental parameters, results into the formation of a highly coloured compound known as 3,4-diaminophenylpiazselenol. The latter is consequently extracted with toluene after making the aqueous solution alkaline, and the colour compared with a standard prepared likewise from a known amount of selenium. The various reactions involved may be expressed as follows ... 

One synthesis approach that does not rely on CNT formation from the gas phase is molten salt synthesis. The reactor consists of a vertically oriented quartz tube that contains two graphite electrodes (i.e. anode is also the crucible) and is filled with ionic salts (e.g. LiCl or LiBr). An external furnace keeps the temperature at around 600 °C, which leads to the melting of the salt. Upon applying an electric field the ions penetrate and exfoliate the graphite cathode, producing graphene-type sheets that wrap up into CNTs on the cathode surface. Subsequently, the reactor is allowed to cool down, washed with water, and nanocarbon materials are extracted with toluene [83]. This process typically yields 20-30 % MWCNTs of low purity. 

As indicated previously, it is important to look at the individual trace elements in the coal extract solution. Table 9 shows the concentration of trace elements in the ash from the original extract and the filtrate produced after toluene extraction. This was for an extract with an ash level of 350 ppm, extracted with toluene at 165 C to give a filtrate with an ash level of 100 ppm. The results show that there are some differences, with Ca reducing and Fe and Ti increasing their proportions. However, the changes are not great and it would be expected that if the filtrate were fed to the hydrocracker it would deposit trace elements as observed previously Q), except, of course, there would be a smaller quantity overall. 

Simulated distillation of the fiaction boiling to 350 C of extract and filtrate after extraction with toluene at 165 C... 

Extraction with toluene containing internal standard... 

The Robinson annulation of ethyl acetoacetate and tra i -chalcone was investigated with pulverized NaOH in [BMIMjPFg as the base catalyst at 100°C 110). The mixture was neutralized before extraction with toluene. The product, 6-ethoxycarbonyl-3,5-diphenyl-2-cyclohexenone, was obtained by purification in a silica gel chromatography column. A yield of 48% was obtained (Scheme 7). The ionic liquid could be recycled and reused with no diminution of product yield. The C2 position in imidazolium cations is an acidic proton donor and may have reacted... 

---