Acetals and Ethers. XVIII. Reaction products of prop-2-enal and but-2-enal with mixture: n-Aliphatic alcohol and ethylene glycol

The direct condensation reaction of prop-2-enal or but-2-enal with mixture of n-aliphatic alcohol and ethylene glycol, in the presence of p-toluenesulphonic acid as catalyst, leads to a complex mixture of saturated, unsaturated, cyclic and linear acetals, moreover, 2-(2-alkoxy-alkyl)-1,3-dioxolanes are the main reaction products. The detailed investigations for n-butanol showed that unsaturated cyclic acetals: 2-vinyl-1,2-dioxolane 1a or 2-(1-propenyl)-1,3-dioxolane 1b , as well as unsaturated linear acetals: 1,1-dibutoxy-prop-2-en 2a or 1,1-dibutoxy-but-2-en 2b are intermediate reaction products. Additionally, it was found in final products presence of eight by-products: 5-butoxy- 4a or 5-butoxy-7-methyl-1,4-dioxepane 4b , 1,1,3-tributoxypropane 5a or 1,1,3-tributoxybutane 5b , 2-[2-(2-hydroxyethoxy)ethyl]- 6a or 2-[2-(2-hydroxyethoxy)propyl]-1,3-dioxolane 6b , 5-(2-hydroxyethoxy)-7-methyl-1,4-dioxepane 7b , 1,3-dibutoxy-1-(2-hydroxyethoxy)-propane 8a or 1,3-dibutoxy-1-(2-hydroxyethoxy)-butane 8b , 1,1-dibutoxy-3-(2-hydroxyethoxy)-propane 9a or 1,1-dibutoxy-3-(2-hydroxyethoxy)-butane 9b , 3-butoxy-1,1-bis-(2-hydroxyethoxy)-propane 10a or 3-butoxy-1,1-bis-(2-hydroxyethoxy)-butane 10b , and 1-butoxy-1,3-bis-(2-hydroxyethoxy)-propane 11a or 1-butoxy-1,3-bis-(2-hydroxyethoxy)-butane 11b , respectively.     

The Reaction of Malononitrile with Enamines of some cyclic β-Keto acid anilides and amidines

The reaction of enamines 1 derivatives of cyclohexanon- or cycloheptanon-2-carboxylic acid anilides with malononitrile gave in the first step 2-phenylcarbamoyl-cycloalkylideno-malononitriles 3 , which in turn were converted into 1-oxo-2-phenyl-3-amino-4-cyano-cycloalkenoisoquinolines 4 . Enamines containing an adjacent diphenylamidino group 6 reacted with malononitrile giving 1-phenylimino-2-phenyl-3-amino-4-cyano-cycloalkenoisoquinolines 7 . The alkaline hydrolysis of 7 yielded 1-phenylamino-3-oxo-4-cyano-cycloalkenoisoquinoline 8 .     

Effect of Antibiotic Amphotericin B Combinations with Selected 1,3,4-Thiadiazole Derivatives on RPTECs in an In Vitro Model

4-(5-methyl-1,3,4-thiadiazole-2-yl) benzene-1,3-diol (C1) and 4-[5-(naphthalen-1-ylmethyl)-1,3,4-thiadiazol-2-yl] benzene1,3-diol (NTBD) are representative derivatives of the thiadiazole group, with a high antimycotic potential and minimal toxicity against normal human fibroblast cells. The present study has proved its ability to synergize with the antifungal activity of AmB. The aim of this work was to evaluate the cytotoxic effects of C1 or NTBD, alone or in combination with AmB, on human renal proximal tubule epithelial cells (RPTECs) in vitro. Cell viability was assessed with the MTT assay. Flow cytometry and spectrofluorimetric techniques were used to assess the type of cell death and production of reactive oxygen species (ROS), respectively. The ELISA assay was performed to measure the caspase-2, -3, and -9 activity. ATR-FTIR spectroscopy was used to evaluate biomolecular changes in RPTECs induced by the tested formulas. The combinations of C1/NTBD and AmB did not exert a strong inhibitory effect on the viability/growth of kidney cells, as evidenced by the negligible changes in the apoptotic/necrotic rate and caspase activity, compared to the control cells. Both NTBD and C1 displayed stronger anti-oxidant activity when combined with AmB. The relatively low nephrotoxicity of the thiadiazole derivative combinations and the protective activity against AmB-induced oxidative stress may indicate their potential use in the therapy of fungal infections.     

Investigation of the structure of poly(p-chlorophenyl glycidyl ether) by the 13C n.m.r. technique: tacticity and addition isomerism

The p-chlorophenyl glycidyl ether was polymerized in the presence of Al(OiPr)₃, ZnCl₂, SnCl₄, BuOK, KOH and by the Al(OiPr)₃ZnCl₂ 1:1 initiator system. Analysis of the ¹³C n.m.r. spectra of the poly(p-chlorophenyl glycidyl ethers) obtained has made it possible to determine their tacticity and the content of the head-to-tail and head-to-head linkages in the polymer chain.     

Monte Carlo simulation of radiation-induced solid state polymerization

A Monte Carlo method was used for a computer simulation of radiation-induced solid state polymerization. The propagation of polymer chains was simulated by means of self-avoiding random walks on a tetrahedral lattice. The initiation and termination of the chains were modelled by pseudorandom processes. The influence of conditions of the in-source process on the post-polymerization kinetics and on the degree of polymerization of the polymers was studied.     

Determination of the ash yield and the mineral matter content of brown coals by density measurements

A method of measuring the density of bed-moist brown coals based on their plastic properties is described and the feasibility of using the method for determination of the ash yield of the coal is evaluated.     

Integrated instrumental analysis of soft brown coals

A method for the simultaneous determination of calorific value Q^r, ash yieldA^r and total water content W^r_t of soft brown coals is described. The method involves instrumental analysis of brown coal samples using neutron thermalization and gamma back-scattering techniques. Over 80 coal samples (1.1 kg) were analysed, having Q^rvalues up to 15.5 MJ kg^?1,A^r ranging from 3.6 to 76.1 wt% and W^r_t ranging from 11.4 to 61.7 wt%. A comparison of the results from the instrumental method with those of standard laboratory analyses is given, followed by a discussion of the accuracy of the method and of possible ways for improving it.     

Process analysis and optimisation of hybrid processes for the dehydration of ethanol

Promising hybrid processes for ethanol dewatering consist of different combinations of distillation with adsorption and/or vapour permeation. This paper presents an analysis and optimisation of these hybrid processes using non-equilibrium models and an evolutionary algorithm. Four different membrane assisted configurations are compared with a benchmark process consisting of distillation and pressure swing adsorption. In total 12 cases were investigated while assuming different feed and product compositions at different production capacities: three ethanol mass fractions in feed 45, 80, 92 wt.%, two product purities 99.6, 99.95 wt.% and two production capacities 25,000, 250,000 m³/year. The influence of decisive operating and structural variables on important target variables such as total membrane area is demonstrated. Finally, the processes are evaluated regarding operating costs and energy consumption depending on product purity and production capacity. The operating costs of the membrane assisted configurations differ only in a small range of −3% to 6% from those of the benchmark. The energy consumption of the membrane assisted configurations without distillation is up to 30% lower compared to the benchmark. Especially the combination of vapour permeation and adsorption is a promising alternative allowing for producing ethanol with high purities at lower operating pressures compared to the vapour permeation as stand alone process.     

The effect of scale and interfacial tension on liquid–liquid dispersion in in-line Silverson rotor–stator mixers

The effect of scale, processing conditions, interfacial tension and viscosity of the dispersed phase on power draw and drop size distributions in three in-line Silverson rotor–stator mixers was investigated with the aim to determine the most appropriate scaling up parameter. The largest mixer was a factory scale device, whilst the smallest was a laboratory scale mixer. All the mixers were geometrically similar and were fitted with double rotors and standard double emulsor stators. 1 wt.% silicone oils with viscosities of 9.4 mPa s and 339 mPa s in aqueous solutions of surfactant or ethanol were emulsified in single and multiple pass modes. The effect of rotor speed, flow rate, dispersed phase viscosity, interfacial tension and scale on drop size distributions was investigated.