Acetonitrile, solution preparation

Compound 9 has been prepared by the latter authors using triethylene glycol diiodide and triethylene glycol diamine (see Eq. 4.11) and an alkali metal carbonate in acetonitrile solution. ... 

Sulfur tetrafluoride, SF4, though extremely reactive (and valuable) as a selective fluorinating agent, is much more stable than the lower fluorides. It is formed, together with SFg, when a cooled film of sulfur is reacted with F2, but is best prepared by fluorinating SCI2 with NaF in warm acetonitrile solution ... 

This group of compounds is represented by A-methyl-2,5-diphenyl-l-aza-6-oxa-6fl-tellurapentalene 94 which was prepared in low yield (11%) by coupling an imidoyl chloride 95 with a tellurenyl chloride 96 in acetonitrile solution containing 2,6-lutidine (87MI2). 

In an initial step, the sodium derivative of ethyl (3-benzoylphenyl)cyanoecetate is prepared as follows (3-benzoylphenyl)acetonitrile (170 g) is dissolved in ethyl carbonate (900 g). There is added, over a period of 2 hours, a sodium ethoxide solution [prepared from sodium (17.7 g) and anhydrous ethanol (400 cc)], the reaction mixture being heated at... 

A bicyclo[3.3.0]octane ring system 164 can be conveniently prepared by refluxing an acetonitrile solution of the azo compound 163 in the presence of excess of phenyl vinyl... 

ET-IR spectroscopy was employed to investigate the structures of the 1 1 complexes between Li" and the guanidine-substituted azo compounds pyiidine-2-azo-p-phenyltetramethylguanidine and 4,4 -bis(tetramethylguanidine)azoben-zene. Both Li" complexes exist as dimers in acetonitrile solution.The structural chemistry of potassium N,N -di(tolyl)formamidinate complexes has been investigated in detail. These compounds were prepared by deprotonation of the parent Af,N -di(tolyl)formamidines with potassium hydride (Scheme 13). The resulting adducts with either THE or DME display one-dimensional polymeric solid-state structures that exhibit /r-fj fj -coordinated formamidinates. 

Prohexadione-calcium standard solutions Dissolve 10 mg of prohexadione-calcium in 100mL of water to prepare a lOOmgL" solution. Transfer 100 p.L of this solution into a 30-mL test-tube, evaporate water to dryness under reduced pressure and to methylate prohexadione-calcium according to Section 6.3. Dissolve the product in acetonitrile to prepare the 0.05,0.2,0.4,0.6 and 0.8 mgL acetonitrile solutions. 

Stock solution. Prepare a 200- ug mL stock solution in ACN Fortification solutions. Prepare 0.04 and 0.2 lagmL fortification solutions by dilution of the stock solution in acetonitrile (trinexapac-ethyl). Prepare 0.05 and 0.25 j.gmL fortification solutions by dilution of the stock solution in water (trinexapac). 

PDPH is soluble in 0.1 M sodium acetate, pH 5.5, at a maximal concentration of 14.2 mg/ml. The reagent is particularly stable in acetonitrile for preparation of concentrated stock solutions. 

By introducing redox-active N-methyl-4,4/-bipyridinium ion (mbpy+) to the oxo-centered triruthenium cores, a series of triruthenium derivatives bearing two or three axially coordinated mbpy+ were prepared by Abe et al. [12, 13]. Electrochemical studies indicated that these mbpy+-containing triruthenium complexes afforded a total of seven to nine reversible or quasi-reversible redox waves in acetonitrile solutions at ambient temperature. Of these redox waves, four or five one-electron redox processes arise from RU3 -based oxidations or reductions involving five or six formal oxidation states, including... 

Metal dithiophosphinato complexes are usually prepared by metathesis of metal halides with alkali metal or ammonium dithiophoshinates, but can also be conveniently prepared by reactions of /i .v(thiophosphinyl)disul fanes, R2(S)PSSP(S)R2, with metal species.87 The electrochemical oxidation of metals in acetonitrile solution, in the presence of diphenylphosphine and sulfur affords M(S2PPh2)2 (M = Co, Zn, Cd),88 but this is not a preparative method. 

An unconventional preparation of nickel diphenyldiselenophosphinate, Ni(Se2 PPh2)2, involves oxidation by elemental selenium of Ni(PPh2)2, obtained in turn by electrochemical oxidation of nickel metal in acetonitrile solutions of PhzPH.449... 

Next, some special methods for preparing organotinhalides are presented. 1,2-Dichlorotetraalkyldistannanes ClR2SnSnR2Cl (R = Me, Et, Bu) have been prepared by the electrolysis of acetonitrile solutions of the appropriate dialkyltin dichloride using... 

N,4,4-Trimethyl-2-oxazolinium iodide is prepared by adding 49.5 g. (0.5 mole) of 4,4-dimethyl-2-oxazoline to an excess of cold methyl iodide (182 g., 80 ml., 1.28 moles) in a 500-ml. flask and stirring at room temperature under argon for 20 hours. The light brown solid is filtered with the aid of suction and then dissolved in 350 ml. of dry acetonitrile. The methiodide salt is precipitated by the addition of 750 ml. of dry ether to this acetonitrile solution. The purified salt is again filtered with the aid of suction, and the white solid is washed with 250 ml. of dry ether and finally dried under vacuum. This gives 96 g. (80%) of the methiodide, m.p. 215° (dec.). 

As a measure of their thermodynamic stability, the pAfR+ values for the carbocation salts were determined spectrophotometrically in a buffer solution prepared in aqueous solution of acetonitrile. The KR+ scale is defined by the equilibrium constant for the reaction of a carbocation with water molecule (/CR+ = [R0H][H30+]/[R+]). Therefore, the larger p/CR+ index indicates higher stability for the carbocation. However, the neutralization of these cations was not completely reversible. This is attributable to instability of the neutralized products. The instability of the neutralized products should arise from production of unstable polyolefinic substructure by attack of the base at the aromatic core. 

The chemical oxidation of 1,3,5-triarylformazans to tetrazolium salts was first accomplished in 1894 [127], Almost no attention was given to these compounds for about 50 years after their discovery. This situation began to alter markedly because of the application of tetrazolium salts in histochemical, pharmacological, and other biomedical research areas [128]. Specifically, the tetrazolium salt is reduced to a colored formazan derivative by reducing enzymes found only in metabolically active cells. Anodic transformation of for-mazans to tetrazolium salts was performed in acetonitrile solution using cotrolled potential electrolysis [17,129], In our view this reaction could be considered as a method of choice for the preparation of tetrazolium salts. The products were obtained in high yield and the electrolysis can be performed in a divided cell under constant current and decoloration of the solution indicates the end point of the reaction. Recently the anodic oxidation of formazans to tetrazolium salts was performed successfully in aqueous ethanol solution [130]. 

Upon addition of perchlorate ions to the acetonitrile solutions, the salt [(MeCN)2ln Mn(C0)j 2]C104 can be isolated. This will react with pyridine or phenanthroline to yield [L2ln Mn(C0)5 2]C104 (L = py or phen). The compounds R4N[X4 In Mn(CO)5)J (n = 1—3 R = Me, X = Cl R == Et, X = Br) have also been prepared. Thus this work shows that as well as influencing the amount of dissociation of metal-metal bonded complexes, the nature of the solvent also determines the mode of ionization. The complex [TljMnlCOljlj] can be conveniently prepared from thallium(i) salts and [Na(Mn(CO)g ]. ... 

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