Organic Components of Moxa

1988 ◽  
Vol 16 (03n04) ◽  
pp. 179-185 ◽  
Author(s):  
Kazuko Kobayashi
Keyword(s):  
Melting Point ◽  
Condensed Tannins ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Mixed Solvent ◽  
Water Layer ◽  
High Class ◽  
Chloroform Layer ◽  
Supernatant Solution ◽  
C Nmr

Moxa was soaked in a mixed solvent of chloroform, menthanol and water (5:5:1) at room temperature for 7 days, and the supernatant solution was seperated into two layers by the addition of water. Heptatriacontane (C37H76), confirmed by measurements of 1H and 13C-NMR spectra and melting point, was obtained from the chloroform layer, while condensed tannins having catechol derivatives were found in the methanol-water layer. Each ratio of C37H76 in several kinds of moxas to the total weight of the moxa was similiar in both high-class and low-class moxas, but that of the tannins was much less in the former than the latter. Comparing the burning-temperature from 25°C to the highest temperature was longer in the treated moxa. Removal of C37H76 from the original moxa seems to decelerate the burning of moxa.

Metall-π-Komplexe yon Benzolderivaten, XIII Bis(methylthio-η-beiizol)chrom(0) Darstellung und Einsatz als zweizähniger Chelatligand/ Metal-π Complexes of Benzene Derivatives, XIII Bis(methylthio-η-benzene)chromium(0) Preparation and Function as a Bidentate Chelating Ligand

1981 ◽  
Vol 36 (1) ◽  
pp. 94-101 ◽  
Author(s):  
Helmut Burdorf ◽  
Christoph Eischenbroich
Keyword(s):  
Nmr Spectra ◽  
Room Temperature ◽  
Radical Cations ◽  
Esr Spectra ◽  
Benzene Derivatives ◽  
Consecutive Reaction ◽  
H Nmr ◽  
Chelating Ligand ◽  
And Function ◽  
C Nmr

Abstract The thioanisole-π-complexes (methylthio-η-benzene)-(η-benzene)-chromium (2) and bis(methylthio-η-benzene)chromium (3) have been prepared via lithiation of bis(η-benzene)-chromium and consecutive reaction with dimethyldisulfide. 1H NMR and 13C NMR spectra of 2 and 3 as well as ESR-spectra of the corresponding radical cations 2.+ and 3.+ were recorded and analyzed. In contrast to C(η-arene)-Si and C(η-arene)-P bonds, C(y-arene)-S bonds are stable to solvolysis. With (norbornadiene)tetracarbonylmolybdenum, 3 readily forms [bis(methylthio-η-benzene)chromium]tetracarbonylmolybdenum (6) wherein 3 functions as a chelating ligand. 1H and 13C NMR evidence suggests, that at room temperature 6 undergoes rapid conformational interconversions.

Substituenteneinflüsse auf Synthese und Eigenschaften von Hexakis[phosphanaurio(I)]methanium(2+)bis(tetrafluoroboraten) / Substituent Effects in Synthesis and Properties of Hexakis[phosphineaurio(I)]methanium(2 +) Bis(tetrafluoroborates)

1992 ◽  
Vol 47 (12) ◽  
pp. 1725-1735 ◽  
Author(s):  
Hubert Schmidbaur ◽  
Benno Brachthäuser ◽  
Siegfried Gamper ◽  
Annette Schier ◽  
Oliver Steigelmann
Keyword(s):  
Nmr Spectra ◽  
Room Temperature ◽  
Substituent Effects ◽  
Reaction Times ◽  
Phosphine Ligands ◽  
Electronic Effects ◽  
X Ray ◽  
Magnetic Resonance Parameters ◽  
Interstitial Carbon Atom ◽  
C Nmr

Polyaurated carbon complexes of the type [(L–Au)6C]2+ with functionalized phosphine ligands have been prepared by the reaction of the phosphinegold(I) chlorides R(Ph)2PAuCl (R = p-C6H4-Cl 2a,p-C6H4-Br 2b,p-C6H4-CH3 2c,p-C6H4-OCH3 2d,p-C6H4-COOH 2e, p-C6H4–N(CH3)2 2f), R2(Ph)PAuCl (R = p-C6H4-N(CH3)2 2g) and R3PAuCl (R = p-C6H4-N(CH3)2 2h) with tetrakis(dimethoxyboryl)methane in HMPT at room temperature. Clearly depending on the different inductive and mesomeric effects, the preparation of the clusters with substituents like –CH3 3c, –OCH3 3d and –N(CH3)2 3f needs shorter reaction times and the products show better solubility in organic solvents than those with functional groups like –Cl 3a, –Br 3b and –COOH 3e. The 31P magnetic resonance parameters are correlated with electronic effects of the substituents, but the chemical shift of the interstitial carbon atom in the 13C-NMR spectra is largely independent of the coordinating ligands. For the phosphinegold(I) chlorides 2f–h X-ray structure analyses have been performed.

Reassignment of the structure of M3(CO)12(Cl)(SnCl3) (M = Ru, Os)

1989 ◽  
Vol 67 (7) ◽  
pp. 1236-1238 ◽  
Author(s):  
Anna Becalska ◽  
Roland K. Pomeroy ◽  
William A.G. Graham
Keyword(s):  
Nmr Spectroscopy ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Quantitative Yield ◽  
Nmr Spectrum ◽  
C Nmr

Reaction of M3(CO)12 (M=Ru, Os) with SnCl4 in benzene at room temperature affords M3(CO)12(Cl)(SnCl3) in essentially quantitative yield. The 13C nmr spectra of these complexes indicate they have a ClM3(SnCl3) arrangement of atoms with the Cl ligand cis and the SnCl3 group trans to a linear Os3 chain. This is contrary to previously proposed structures for these compounds. The 13C nmr spectrum of Os3(CO)12(I)2 which has the iodo ligands cis to the Os3 chain is also reported for comparison. Keywords: ruthenium–tin, osmium–tin, osmium–iodine, l3C nmr spectroscopy.

1,4-Bis(p-pentazolylphenyl)butan, 1-p-Azidophenyl-4-p-pentazolylphenyl- butan und 1,4-Bis(p-azidophenyl)butan / 1,4-Bis(p-pentazolylphenyl)butane, 1-p-Azidophenyl-4-p-pentazolylphenyl-butane and 1,4-Bis(p-azidophenyl)butane

2004 ◽  
Vol 59 (6) ◽  
pp. 716-720 ◽  
Author(s):  
Frank Biesemeier ◽  
Klaus Harms ◽  
Ulrich Müller
Keyword(s):  
Low Temperature ◽  
Sodium Azide ◽  
Rate Constants ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Fine Powder ◽  
Space Group ◽  
H Nmr ◽  
Diazonium Ions ◽  
C Nmr

1,4-Bis(p-pentazolylphenyl)butane (1), 1-p-azidophenyl-4-p-pentazolylphenyl-butane (2) and 1,4-bis(p-azidophenyl)butane (3) were obtained by the reaction of 1,4-diphenylbutane-4’,4”- bis(diazonium) ions with sodium azide in methanol at −50 °C. In the 1H and 13C NMR spectra the three compounds can be distinguished unequivocally. At −50 °C a mixture with a composition 1:2:3 of 10:30:60 was obtained. By recrystallization first from dichloromethane/methanol and then from dichloromethane/petroleum ether the pentazole components were enriched to a composition ratio of 21:62:17. The rate constants of the decompositions 1→2 and 2→3 at 0 °C were determined from the variation of the 1H NMR intensities. At room temperature all of the material is converted to 3. 3 crystallizes in two monoclinic modifications. At −70 °C a modification 3-LT having space group P21/c (a = 950.8, b = 1192.6, c = 701.3 pm, β = 92.55°, Z = 2; R = 0.075) was obtained. The modification crystallizing at room temperature (3-HT) has space group I2/a (a = 1514.5, b = 498.1, c = 2027.9 pm, β = 92.73°, Z = 4; R = 0.040). Whereas both modifications consist of nearly identical molecules, their packings are quite different. When the low temperature modification is warmed to room temperature, its crystals jump like flees and are disrupted to a fine powder.

Ein weiteres P-Fluor-Ylid: [N(CH3)2]2PF=CH-CH(n-C4H9)-P[N(CH3)2]2 (4) Darstellung und NMR-Daten / A Further P-Fluoro-Ylide: [N(CH3)2]2 PF=CH-CH(n-C4H9)-P[N(CH3)2] 2 (4) Preparation and NMR Data

1987 ◽  
Vol 42 (3) ◽  
pp. 260-266 ◽  
Author(s):  
Gernot Heckmann ◽  
Bernhard Neumüller ◽  
Ekkehard Fluck
Keyword(s):  
Long Range ◽  
Title Compound ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Resonance Mode ◽  
Triple Resonance ◽  
Hindered Rotation ◽  
Nmr Data ◽  
C Nmr

Preparation and properties of the title compound 4, [N(CH3)2]2 PF2-(CH2)2-PF2[N(CH3)2]2 (2), and [N(CH3)2]2+PF-(CH2)2--PF5 (3), are described. The 1H, 19F, 31P, and 13C NMR spectra in double and triple resonance mode of 4 are recorded and discussed in detail. A 7J(HF) long-range coupling could be identified. 300 MHz-1H spectra show hindered rotation around the P-N bonds at room temperature

The Preparation of Some Mono-and Bis(thiolate)-2-butyne Complexes of Tungsten(II) of the Types [WI(SR)(CO)(dppm )(η2-MeC2Me)] {dppm = Ph2P(CH2)PPh2; R = Et, But, Ph or CH2Ph} and [W (SR)2(CO)(dppm)(η2-MeC2Me)]

1994 ◽  
Vol 49 (11) ◽  
pp. 1544-1548 ◽  
Author(s):  
Paul K. Baker ◽  
Kevin R. Flower
Keyword(s):  
Nmr Spectroscopy ◽  
Elemental Analysis ◽  
Good Yield ◽  
Nmr Spectra ◽  
Room Temperature ◽  
H Nmr ◽  
Thiolate Complexes ◽  
C Nmr

Equimolar quantities of [WI(CO)(NCMe)(dppm)(η2-MeC2Me)][BF4] {dppm = Ph2P(CH2)PPh2) and NaSR (R = Et. But ,Ph or CH2Ph) react in CH2Cl2 at room temperature to give the neutral thiolate complexes [WI(SR)(CO)(dppm)(η2-MeC2Me)] (1 → 4) in good yield. The complex [WI(CO)(NCMe)(dppm)(η2-MeC2Me)][BF4] also reacts with two equiv­alents of NaSR (R = Et. But, Ph or CH2Ph) in CH2Cl2 at room temperature to afford the bis(thiolate) complexes [W(SR)2(CO)(dppm)(η2-MeC2Me)] (5 → 8), in good yield. Com­plexes 1→8 have been characterized by elemental analysis (C, H and N), IR and 1H NMR spectroscopy. 13C NMR spectra of selected complexes indicate that the 2-butyne ligand is donating four electrons to the metal in both [WI(SR)(CO)(dppm)(η2-MeC2Me)] and [W(SR)2(CO)(dppm)(η2-MeC2Me)] type complexes.

scholarly journals A New Triglycosyl Flavonoid Isolated from Leaf Juice of Kalanchoe gastonis-bonnieri (Crassulaceae)

2015 ◽  
Vol 10 (3) ◽  
pp. 1934578X1501000 ◽  
Author(s):  
Sônia Soares Costa ◽  
Maria Fernanda Paresqui Corrêa ◽  
Livia Marques Casanova
Keyword(s):  
Nmr Spectra ◽  
Room Temperature ◽  
Structural Elucidation ◽  
Phytochemical Study ◽  
First Report ◽  
Flowering Season ◽  
Flavonoid Quercetin ◽  
Leaf Juice ◽  
Genitourinary Infections ◽  
C Nmr

Kalanchoe gastonis-bonnieri R. Hamet & H. Perrier (Crassulaceae) is a succulent species empirically used as a vaginal contraceptive as well as to heal genitourinary infections. A phytochemical study of leaf juice prepared from specimens collected in the flowering season resulted in the isolation of the new flavonoid quercetin 3- O-α-rhamnopyranoside-7- O-β-D-glucopyranosyl-(1→3)-α-L-rhamnopyranoside, as well as the already known 6- C-β-D-glucopyranosyl-8- C-β-D-glucopyranosylapigenin (vicenin-2). The NMR spectra of this flavonoid at room temperature exhibited broad and duplicated signals, suggesting the existence of rotameric conformers, which was confirmed by coalescence of the signals at 40°C. The structural elucidation was based on 1H and 13C NMR (HMQC and HMBC) analyses and MS data. This is the first report of a C-glycosyl flavonoid (vicenin-2) in the Crassulaceae family. Additionally, this is the first study in which atropoisomerism has been shown for vicenin-2.

NMR-Untersuchungen an 3,3-Difluor-2-ethyI-1,1,2-tris(diethoxyphosphoryI)-cyclopropan / NMR Investigation of 3,3-Difluoro-2-ethyl-1,1,2-tris(diethoxyphosphoryl)cyclopropane

1986 ◽  
Vol 41 (1) ◽  
pp. 63-69 ◽  
Author(s):  
Gernot Heckmann ◽  
Ekkehard Fluck ◽  
Jürgen Svara
Keyword(s):  
Temperature Dependence ◽  
Title Compound ◽  
Nmr Spectra ◽  
Room Temperature ◽  
Resonance Mode ◽  
Triple Resonance ◽  
The Third ◽  
Nmr Parameters ◽  
Phosphoryl Groups ◽  
C Nmr

The 19F, 31P and 13C NMR spectra in double and triple resonance mode and the temperature dependence of the NMR parameters of the title compound are discussed in detail. The rotational behavior of the phosphoryl groups is described; two of these groups show equal barriers to rotation of 75 kJ mol-1, the third one is rotating freely at room temperature.

Stability and decarbonylation of 1,3-dialkyl-2-formylimidazolium perchlorate in solution

2013 ◽  
Vol 91 (6) ◽  
pp. 442-447 ◽  
Author(s):  
Hong-Xing Xin ◽  
Qi Liu ◽  
Hong Yan ◽  
Xiu-Qing Song
Keyword(s):  
Nmr Spectra ◽  
Room Temperature ◽  
X Ray ◽  
H Nmr ◽  
Protic Solvents ◽  
The Stability ◽  
C Nmr

The stability of 1,3-dialkyl-2-formylimidazolium perchlorate 1 in solution was studied in detail and found to be related to its structure and the solvent character and temperature. 1 was stable in common solvents at room temperature and unstable in protic solvents under reflux. In protic solvents, such as H2O, MeOH, EtOH, and AcOH, 1 decarbonylated into 1,3-dialkylimidazole perchlorates 2, which was confirmed by 1H NMR, 13C NMR, HRMS, and X-ray spectroscopy. The decarbonylation of 1 was proposed to occur via its hemiacetal formed by the addition of solvents based on the tracking NMR spectra of 1 in deuterated reagents.

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