Proton and carbon-13 nuclear magnetic resonance studies of the conformational properties of seven-membered heterocycles. 2,4-Benzodithiepin and its derivatives

1979 ◽  
Vol 57 (24) ◽  
pp. 3221-3229 ◽  
Author(s):  
F. Sauriol-Lord ◽  
M. St-Jacques
Keyword(s):  
Membered Ring ◽  
Steric Effects ◽  
Axial Position ◽  
Minor Amount ◽  
Equatorial Position ◽  
Stable Conformation ◽  
Magnetic Resonance Studies ◽  
Conformational Effect ◽  
Conformational Properties ◽  
A Minor

The conformational properties of 1,3-dithia-5,6-benzocycloheptene (7) (2,4-benzodithiepin), three 2,2-dialkyl derivatives, and two monosubstituted derivatives (2-CH3 and 2-OCH3) have been investigated by 1H and 13C dnmr methods. It is reported that the most stable conformation of the seven-membered ring is a chair on which, in the case of the monosubstituted compounds, the 2-CH3 group adopts an equatorial position while the 2-OCH3 group takes the axial position. Only for the 2,2-pentamethylene derivative (10) was a minor amount (13%) of TB form detected. These results are markedly different from those found previously for the oxygen analogs and the conformational effect of the cyclic heteroatoms will be discussed in terms of the anomeric and steric effects.

scholarly journals Odour-active compounds in liquid malt extracts for the baking industry

2021 ◽  
Author(s):  
Nadine S. Rögner ◽  
Veronika Mall ◽  
Martin Steinhaus
Keyword(s):  
Threshold Value ◽  
Starting Material ◽  
Minor Amount ◽  
Malt Extract ◽  
Important Process ◽  
Gas Chromatography Olfactometry ◽  
Odour Threshold ◽  
A Minor ◽  
Baking Industry ◽  
Insight Into

AbstractAn odorant screening by gas chromatography–olfactometry (GC–O) and a crude aroma extract dilution analysis (AEDA) applied to the volatiles isolated from a light and a dark liquid malt extract (LME) by solvent extraction and solvent-assisted flavour evaporation (SAFE) identified 28 odorants. Fifteen major odorants were subsequently quantitated and odour activity values (OAVs) were calculated as ratio of the concentration to the respective odour threshold value (OTV). Important odorants in the light LME included 3-(methylsulfanyl)propanal (OAV 1500), (E)-β-damascenone (OAV 430), and 4-ethenyl-2-methoxyphenol (OAV 91). In the dark LME, sotolon (OAV 780), 3-(methylsulfanyl)propanal (OAV 550), (E)-β-damascenone (OAV 410), acetic acid (OAV 160), and maltol (OAV 120) were of particular importance. To get an insight into the changes during malt extract production, the quantitations were extended to the malt used as the starting material for both LMEs. Addition of a minor amount of water to malt before volatile extraction was shown to be effective to cover the free as well as the bound malt odorants. Results showed that some LME odorants originated from the starting material whereas others were formed during processing. Important process-induced LME odorants included (E)-β-damascenone and 4-ethenyl-2-methoxyphenol in the light LME as well as maltol, sotolon, (E)-β-damascenone, and 2-methoxyphenol in the dark LME. In summary, the odorant formation during LME production was shown to be more important than the transfer of odorants from the malt.

Conformational properties of cyclic pentaalkoxy phosphoranes: Apical-equatorial attachment and nonchair conformation of the phosphorus-containing six-membered ring

1991 ◽  
Vol 2 (1) ◽  
pp. 177-185 ◽  
Author(s):  
Jaehoon Yu ◽  
Alan E. Sopchik ◽  
Atta M. Arif ◽  
Wesley G. Bentrude ◽  
G.-V. Roeschenthaler
Keyword(s):  
Membered Ring ◽  
Phosphorus Containing ◽  
Conformational Properties

CLAY-INORGANIC STUDIES. II. HYDROXY ALUMINUM PHOSPHATE–MONTMORILLONITE COMPLEX

1975 ◽  
Vol 55 (2) ◽  
pp. 225-233 ◽  
Author(s):  
H. KODAMA ◽  
M. D. WEBBER
Keyword(s):  
Relative Humidity ◽  
Room Temperature ◽  
Aluminum Phosphate ◽  
Silicate Layer ◽  
Basal Spacing ◽  
Minor Amount ◽  
Chemical Compositions ◽  
A Minor ◽  
Positively Charged ◽  
Water Contents

Two specimens of hydroxy aluminum phosphate interlayer materials in montmorillonite clay were prepared with 7.20 meq Al and 11.29 meq H3PO4/g clay and with 14.40 meq Al and 22.58 meq H3PO4/g clay, and the resulting complexes studied by chemical and mineralogical methods. Both interlayer materials were slightly positively charged and except for different water contents their chemical compositions were almost identical. They contained Al, PO4 and H2O and a minor amount of Ca and approximated hydrous AlPO4∙nH2O. The mole ratios of Al:Ca:PO4:OH were 1.00:0.08:0.92:0.24 and 1.00:0.05:0.91:0.24, respectively. The interlayer materials appeared to be loosely packed and distributed sparsely in interspaces of the montmorillonite. The degree of packing was greater for the preparation with the larger amount of interlayer material. The materials increased the montmorillonite basal spacing to 23.3 Å under air-dry condition (30–40% relative humidity) but did not affect the lateral dimensions. The basal spacing varied somewhat with relative humidity at room temperature and decreased markedly as water was driven off by heating. Heat treatments between room temperature and 300 C sharply reduced the d001 spacings to 16.7 Å which persisted up to 700 C. It is postulated that the large basal spacings occur because the hydrated interlayer materials have a framework structure with tunnels along the c-axis. This being so, changes in the spacings with different humidities might result from the movement of water molecules among interstitial spaces existing around and between the loosely distributed molecules of interlayer material. The 16.7 Å spacing for the dehydrated phase corresponds to the sum of 7.0 Å, the edge dimension of an orthorhombic anhydrous AlPO4 and 9.7 Å, the silicate layer thickness.

Nuclear magnetic resonance characterization of the ring conformations of monosubstituted derivatives of 1,3-dioxa-5,6-benzocycloheptene

1983 ◽  
Vol 61 (1) ◽  
pp. 109-115 ◽  
Author(s):  
R. St-Amour ◽  
M. St-Jacques
Keyword(s):  
Nuclear Magnetic Resonance ◽  
Magnetic Resonance ◽  
Substituent Effects ◽  
Steric Effects ◽  
Slow Exchange ◽  
Conformational Properties ◽  
Derivatives Of ◽  
Ring Conformations ◽  
Twist Boat

The conformational properties of 2-alkyl (Me, Et, i-Pr, and t-Bu) and 2-phenyl derivatives of 1,3-dioxa-5,6-benzocycloheptene (1) were studied by 13C dnmr. Analysis of slow exchange spectra at 100.6 MHz indicates that all derivatives except tert-butyl exist in an equilibrium of chair (major) and twist-boat (minor) conformations. Substituent effects on the position of the equilibrium are rationalized in terms of steric effects.

scholarly journals Vinyl ether hydrolysis. XIV. 2-Methoxy-2,3-dihydropyran: concurrent reaction of vinyl ether and acetal functional groups

1980 ◽  
Vol 58 (21) ◽  
pp. 2199-2202 ◽  
Author(s):  
R. A. Burt ◽  
Y. Chiang ◽  
A. J. Kresge
Keyword(s):  
Vinyl Ether ◽  
Isotope Effect ◽  
Reaction Rate ◽  
Functional Group ◽  
Minor Amount ◽  
Cyanoacetic Acid ◽  
Buffer Solutions ◽  
Hydrogen Isotope Effect ◽  
A Minor ◽  
Hydrolysis Of

The hydrolysis of 2-methoxy-2,3-dihydropyran shows a normal isotope effect (kH/kD > 1) under catalysis by the hydrogen ion and gives an accurately linear dependence of reaction rate upon undissociated acid concentration in cyanoacetic acid and formic acid buffer solutions. This substrate, therefore, unlike its higher homolog, 9-methoxyoxacyclonon-2-ene, provides no evidence in support of an anything but a normal mechanism for vinyl ether hydrolysis. Analysis of the hydrogen isotope effect suggests that a minor amount (8%) of this hydrolysis occurs via reaction of the acetal functional group.

scholarly journals Silica-Based Composites with Enhanced Rheological Properties Thanks to a Nanosized Graphite Functionalized with Serinol Pyrrole

2021 ◽  
Vol 11 (23) ◽  
pp. 11410
Author(s):  
Gea Prioglio ◽  
Silvia Agnelli ◽  
Stefano Pandini ◽  
Maurizio Galimberti
Keyword(s):  
Rheological Properties ◽  
High Surface ◽  
High Surface Area ◽  
Minor Amount ◽  
Carbon Filler ◽  
Hybrid Filler ◽  
Carbon Efficiency ◽  
Dynamic Rigidity ◽  
A Minor ◽  
New Generation

Silica-based rubber composites have tremendous importance, as they allow the reduction in hysteresis in demanding dynamic-mechanical applications such as tire compounds and hence have a lower environmental impact. However, they also present drawbacks such as poor rheological behavior. In this work, an innovative silica-based hybrid filler system was developed, obtaining a rubber composite with an improved set of properties. A nanosized high surface area graphite (HSAG) was functionalized with 2-(2,5-dimethyl-1H-pyrrol-1-yl)propane-1,3-diol, serinol pyrrole (SP), through a simple process characterized by a high carbon efficiency. The HSAG-SP adduct, with about nine parts of SP per hundred parts of carbon filler, was used to form a hybrid filler system with silica. An elastomeric composite, with poly(styrene-co-butadiene) from anionic polymerization and poly(1,4-cis-isoprene) from Hevea brasiliensis was prepared with 50 parts of silica, which was replaced in a minor amount (15%) by either pristine HSAG or HSAG-SP. The best set of composite properties was obtained with HSAG-SP: the same dynamic rigidity and hysteresis and tensile properties of the silica-based material and appreciably better rheological properties, particularly in terms of flowability. This work paves the way for a new generation of silica-based composites, with improved properties, based on a hybrid filler system with a nanosized edge functionalized graphite.

Combustion synthesis of Si3N4 powder

1997 ◽  
Vol 12 (3) ◽  
pp. 805-811 ◽  
Author(s):  
Wei-Chang Lee ◽  
Shyan-Lung Chung
Keyword(s):  
Reaction Mechanism ◽  
Combustion Synthesis ◽  
Combustion Temperature ◽  
Fine Particles ◽  
Minor Amount ◽  
Synthesis Reaction ◽  
Experimental Parameters ◽  
Combustion Synthesis Reaction ◽  
A Minor ◽  
Low Nitrogen

A combustion synthesis (SHS) process has been developed for the synthesis of Si3N4 powder under low nitrogen pressures. Si and NaN3 powders were used as the reactants, and NH4Cl powder was added as a catalytic agent. These powders were mixed and pressed into a cylindrical compact. The compact was wrapped up with an igniting agent (i.e., Ti + C), and the synthesis reaction was triggered by the combustion of the igniting agent. Addition of NH4Cl was found necessary for the combustion synthesis reaction under low nitrogen pressures (< 1.2 MPa). The product as synthesized is mostly in the form of agglomerated fine particles (0.1–1 μm in diameter) and is composed mainly of α-phase and a minor amount of β-phase. Effects of various experimental parameters (N2 pressure, NaN3, NH4Cl, and Si3N4 contents) on the product conversion and the combustion temperature were investigated. A possible reaction mechanism was proposed that explains the effects of the experimental parameters on the synthesis reaction.

scholarly journals The Abundance Pattern of Elements Having Low Nebular Condensation Temperatures in Interplanetary Dust Particles: Evidence for a New Chemical Type of Chondritic Material

1996 ◽  
Vol 150 ◽  
pp. 291-294 ◽  
Author(s):  
G. J. Flynn ◽  
S. Bajt ◽  
S. R. Sutton ◽  
M. E. Zolensky ◽  
K. L. Thomas ◽  
...  
Keyword(s):  
Solar Nebula ◽  
Interplanetary Dust ◽  
Major Elements ◽  
Dust Particles ◽  
Element Abundance ◽  
Minor Amount ◽  
Interplanetary Dust Particles ◽  
Abundance Pattern ◽  
Refractory Elements ◽  
A Minor

AbstractThe abundances of Ni, Fe, Cr, Mn, P, Cu, K, Na, Ga, Ge, Se, Zn, S, Br, and C were measured in interplanetary dust particles (IDPs) collected from the Earth's stratosphere. All elements with nebular condensation temperatures lower than Mn, except S, were enriched relative to the most volatile-rich type of meteorite while the refractory elements Cr and Ni were present at chondritic abundances. This element abundance pattern is consistent with nebular condensation, suggesting the IDPs condensed at either a different location or time in the evolving solar nebula than do the meteorites. The enrichments of the major elements C, Na, P, and K exclude the possibility that the volatile enrichment in IDPs results from a minor amount of contamination.

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