The singular autocatalytic behaviour of the oxidation of acetic acid by methyltributylammonium permanganate in methylene chloride

Author(s):  
Joaquin F. Perez-Benito
1987 ◽  
Vol 40 (10) ◽  
pp. 1663 ◽  
Author(s):  
J Rosevear ◽  
JFK Wilshire

The reaction of several substituted o- nitronitrosobenzenes with O- and p- anisidine , and 2,4- dimethoxyaniline in acetic acid gives in good yield the corresponding enitroazobenzenes which are readily reduced with thiourea dioxide ( formamidinesulfinic acid) to the corresponding 2-(methoxypheny1)-2H-benzotriazoles, demethylation of which furnished the corresponding 2- (hydroxypheny1)-2H-benzotriazoles. Demethylation of the dimethoxy derivatives was best accomplished with boron tribromide in methylene chloride, the methoxy group located ortho to the benzotriazole ring being demethylated more readily than is the para-methoxy group. The reaction of enitroazobenzenes containing a methoxy group with hydrobromic acid in acetic acid results in cleavage of the azo bond and also partial bromination to give o- nitroaniline and some of its brominated derivatives.


2020 ◽  
Vol 66 (1) ◽  
pp. 23-29
Author(s):  
Octavia-Laura Moldovan ◽  
Diana-Nicoleta Brihan ◽  
Nicoleta Todoran ◽  
Aura Rusu

AbstractObjective: The compatibility of four binary active substances combinations adapalene – levofloxacin (ADP-LFX), adapalene – miconazole nitrate (ADP-MCZ), levofloxacin – meloxicam (LFX-MLX) and levofloxacin – miconazole nitrate (LFX-MCZ) was analysed to be comprised in new transdermal therapeutic systems. Also, the compatibility of selected active substances and four polymeric excipients (hydroxypropyl methyl-cellulose - HPMC 15000, hydroxypropyl methylcellulose - HPMC E5, ethyl cellulose - EC 10, and hydroxyethyl cellulose – HEC) was studied.Methods: Thin layer chromatographic method (TLC) and four selected mobile phases were used. On the plate (in situ) were obtained the binary combinations (active substances and active substance-polymer).Results: A good compatibility of ADP-LFX was found using ammonia : methanol : acetonitrile : methylene chloride 2:4:1:4 mobile phase. Using chloroform : acetone : glacial acetic acid 34:4:3 on the chromatogram of ADP-MCZ, only ADP spots appeared but without changes in the shape of the spots and Rf values. Any modifications of LFX and MLX spots (from LFX-MLX mixture) had been observed using toluene : glacial acetic acid : methanol 11:1:0.5 mobile phase, although LFX spots have remained on the baseline. Only LFX spots were visible from LFX-MLX and LFX-MCZ mixtures (ammonia : methanol : acetonitrile : methylene chloride 2:4:1:4 mobile phase). Distinctive spots were observed for ADP, LFX and MLX with variable results from no chemical interactions to limited chemical interactions when the compatibility with polymers was verified.Conclusions: ADP-LFX and LFX-MLX mixtures were found to be compatible. ADP with HPMC polymers and LFX with HPMC E5 and HEC had presented excellent compatibility; for the other binary combinations, different analytical methods will be necessary.


1965 ◽  
Vol 48 (4) ◽  
pp. 771-774
Author(s):  
D P Johnson ◽  
H A Stansbury

Abstract A method has been developed for detecting residues of carbaryl (1-naphthyl methylcarbamate) as well as its hydrolysis product, 1-naphthol, in dead bees. The method is based on extraction of the bees with benzene, followed by a cleanup involving liquid partitioning and chromatography on Florisil. The quantitative determination involves hydrolysis of carbaryl to 1-naphthol and coupling of the latter with p-nitrobenzenediazonium fluoborate in acetic acid to form a yellow substance. For separate analysis, free 1-naphthol is separated from methylene chloride into a basic aqueous solution. The sensitivity of the method is about 0.1 ppm; recoveries averaged 85.6 ± 6.6% for 1- naphthol and 83.8 ± 2.7% for carbaryl.


1985 ◽  
Vol 40 (5) ◽  
pp. 594-600 ◽  
Author(s):  
Ralf Steudel ◽  
Torsten Sandow ◽  
Jürgen Steidel

Abstract The homocyclic oxides S9O (m.p. 33 °C, dec.) and S10O (m.p. 51 °C, dec.) have been prepared by oxidation of the corresponding sulfur rings S9 and S10 , respectively, by trifluoroperoxy acetic acid (molar ratio 1:2-3) in a carbon disulfide/methylene chloride mixture. According to infrared and Raman spectra, both compounds contain an exocyclic oxygen atom. S9O and S10O decompose at 25 °C to give SO2 and a polysulfuroxide SnO with >10 but both can be stored at -78 °C without decomposition. The SS bond distances are discussed on the basis of the Raman spectra. In addition, the Raman spectrum of solid S9 has been recorded for the first time. It shows that S9 crystallizes as two allotropes (α-and β-S9) both consisting of cyclic molecules of either C1 or C2 symmetry with bond distances of between 203 and 209 pm.


1982 ◽  
Vol 65 (3) ◽  
pp. 659-664 ◽  
Author(s):  
Gerald C Llewellyn ◽  
Thomas Eadie ◽  
William V Dashek

Abstract The susceptibility of blackberries, cherries, and strawberries to Aspergillus growth and aflatoxin production has been examined. Three aflatoxigenic isolates of Aspergillus, A. flavus ATCC 15548 and NRRL 3251 as well as A. parasiticus NRRL 2999, were cultured on homogenates of the fruits for 14 days at 28 ± 2°C. Percent mycelial growth and spore infestation were determined each day with a calibrated grid. At day 14 each culture was frozen at –5°C until aflatoxins were extracted with methylene chloride and water. Aflatoxins were separated by thin layer chromatography (TLC) with benzene-methanol-acetic acid (90 + 5 + 5). This extraction and solvent system provided satisfactory separations of the aflatoxins and was free of background interference on the TLC plates. Although all fruits served as substrates for both Aspergillus growth and aflatoxin production, cherries appeared to be a more favorable substrate than did blackberries, and the latter was more favorable than strawberries. Whereas A. flavus produced both B1 and G1 on all substrates, it yielded B2 and G2 only on cherries. Although A. parasiticus NRRL 2999 synthesized B1, B2, G1, and G2 on both blackberries and cherries, no aflatoxins were detected on strawberries. In contrast, A. flavus NRRL 3251 failed to produce detectable levels of aflatoxin on any substrate. All substrates supported both mycelial growth and subsequent sporulation with cherries > blackberries > strawberries.


1977 ◽  
Vol 55 (3) ◽  
pp. 421-426 ◽  
Author(s):  
J. Stuart Grossert ◽  
William R. Hardstaff ◽  
Richard F. Langler

Details are provided of synthetic routes from dialkyl sulfides to both α-halosulfoxides and sulfinyl chlorides. In the case of the former, oxidation of α-halosulfides to the sulfoxide stage is achieved by chlorine in acetic acid containing controlled amounts of water. Sulfinyl chlorides are prepared by chlorination of α-polyhalosulfoxides in methylene chloride. During investigations into the details of the sulfohaloform reaction, a number of novel redox reactions involving oxygen transfer between sulfur species have been observed and these are presented. They include a reduction of a sulfoxide with thionyl chloride.


1990 ◽  
Vol 68 (1) ◽  
pp. 79-81 ◽  
Author(s):  
Joaquin F. Perez-Benito ◽  
Enrique Brillas ◽  
Conchita Arias

An iodimetric technique has been developed to quantitatively analyze the oxidants present in organic solutions. Addition of excess tetrabutylammonium iodide and excess glacial acetic acid results in the formation of tetrabutylammonium triiodide, whose concentration can be measured spectrophotometrically at 295 or 365 nm. Application of this technique to the determination of the final oxidation state of manganese in permanganate reactions in methylene chloride solutions is described. The equilibrium constant for formation of tetrabutylammonium triiodide in methylene chloride has been measured: K = (3.48 ± 0.12) × 104 at 25.0 °C. Keywords: iodimetric determinations, manganese oxidation states, methylene chloride, quaternary ammonium permanganate, quaternary ammonium triiodide.


1972 ◽  
Vol 50 (24) ◽  
pp. 3988-3992 ◽  
Author(s):  
Alfred Fischer ◽  
Alan Leslie Wilkinson

cis and trans isomers of 1,4-dimethyl-4-nitro-1,4-dihydro-1-naphthyl acetate (1) have been isolated from a mixture of 1,4-dimethylnaphthalene and nitric acid in acetic anhydride by quenching at −40°. At room temperature only 1-methyl-4-nitromethylnaphthalene (4) is obtained. The conversion of 1,4-dimethylnaphthalene to 4 and of the cis (1a) and trans (1b) adducts to 4, by nitric acid in acetic anhydride, has been followed by n.m.r. 1,4-Dimethyl-4-nitro-1,4-dihydro-1-naphthyl nitrate (5) appears to be the immediate product from nitration of 1,4-dimethylnaphthalene in acetic anhydride, methylene chloride, or nitromethane. In acetic anhydride 5 is converted into 1. Decomposition of 1 in acetic acid gives 1,4-dimethyl-2-naphthyl acetate and some 4. The formation of 4 in this reaction is suppressed by urea.


2011 ◽  
Vol 2011 ◽  
pp. 1-10 ◽  
Author(s):  
A. Gholipour Kanani ◽  
S. Hajir Bahrami

Polycaprolactone nanofibers were prepared using five different solvents (glacial acetic acid, 90% acetic acid, methylene chloride/DMF 4/1, glacial formic acid, and formic acid/acetone 4/1) by electrospinning process. The effect of solution concentrations (5%, 10%, 15% and 20%) and applied voltages during spinning (10 KV to 20 KV) on the nanofibers formation, morphology, and structure were investigated. SEM micrographs showed successful production of PCL nanofibers with different solvents. With increasing the polymer concentration, the average diameter of nanofibers increases. In glacial acetic acid solvent, above 15% concentration bimodal web without beads was obtained. In MC/DMF beads was observed only at 5% solution concentration. However, in glacial formic acid a uniform web without beads were obtained above 10% and the nanofibers were brittle. In formic acid/acetone solution the PCL web formed showed lots of beads along with fine fibers. Increasing applied voltage resulted in fibers with larger diameter.


1981 ◽  
Vol 64 (5) ◽  
pp. 1055-1059
Author(s):  
Wray Winterlin ◽  
Gregory Hall ◽  
Charles Mourer

Abstract A simple and sensiiive procedure is presented for the I determination of furazolidone in turkey tissues, j using liquid partitioning followed by high performance liquid chromatography (HPLC). Fat, liver, kidney, skin, and muscle tissues are ground with methylene chloride in a Polytron homogenizer, followed by solvent removal, partitioning in hexane-0.01M acetic acid, and back-partitioning the 0.01M acetic acid with methylene chloride. The determination by HPLC used a reverse phase Ultrasphere- ODS 5 μm column. The method is sensitive to 0.5 ppb, with a standard deviation of 6.39% at the 2 ppb fortification level. Recovery from fortified tissues j averaged 84% from samples fortified with 0.5-10 ppb furazolidone. An alternative cleanup procedure I using a Sep-Pak C18 cartridge is also presented.


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