Senecicannabine,a new pyrrolizidine alkaloid from senecio cannabifolius

The structure of senecicannabine($\text{1}$), a new mcrocyclic pyrrolizidine alkaloid isolated from $\text{Senecio cannabifolius}$, has been established by chemical study and X-ray analysis.     

Vacuum fusion determination of micro-quantities of bulk gases in low carbon iron without an effect of surface gases

Summary Vacuum Fusion Determination of Micro-quantities of Bulk Gases in Low Carbon Iron Without an Effect of Surface Gases Micro-quantities of bulk and surface oxygen and hydrogen in low carbon iron was simultaneously determined by the surface-area-variation method using vacuum fusion analysis. Among the difference of three surface treatments, silicon carbide abrasive, electropolishing and hydrogen reduction methods, bulk oxygen and hydrogen were in agreement within their errors, however, surface oxygen and hydrogen were influenced from the surface treatments. Even in the case of electropolishing, which gave the smallest surface oxygen value, bulk oxygen less than 10g/g is needed to discriminate from the surface oxygen. Bulk hydrogen of 0.03g/g was determined without the effect of surface hydrogen in the hydrogen reduction treatment.     

Manganese(II) o ctacyanotungstate(V)-based magnet containing a noncoordinated aromatic molecule

We have prepared a pillared layer magnetic material containing a noncoordinated aromatic molecule, [{MnII(pyrimidine)(H2O)}2{MnII(H2O)2}{WV(CN)8}2](pyrimidine)2.2H2O. This compound has one-dimensional channels (6.2 x 2.1 A) that are occupied by noncoordinated pyrimidine. The magnetization versus temperature plots showed the magnetic phased transition temperature (TC) was 47 K. The magnetization versus external magnetic field plots showed that the saturation magnetization (MS) value was 13.0 muB at 2 K. This MS value indicates that an antiferromagnetic interaction operates between the WV (S = 1/2) and MnII (S = 5/2) ions. The magnetic hysteresis loop showed that the coercive field (HC) was 17 G at 2 K.     

The electrochemical behavior of ad-atoms and their effect on hydrogen evolution: Part II. Arsenic ad-atoms on platinum

The state of an arsenic layer electrodeposited at various potentials on platinum electrodes has been examined electrochemically. The relation between the state and the electrocatalytic activity for hydrogen evolution has been investigated. The number of vacant sites have been found to increase with lowering of the deposition potential. The activity has been found to depend not on the amount of deposited arsenic but on the number of vacant sites. The difference in the effects of arsenic and of copper on hydrogen evolution is pointed out. This is attributed to the difference in the affinity of the ad-atoms for hydrogen.     

Enteric solid dispersion of ciclosporin A (CiA) having potential to deliver CiA into lymphatics

Solid dispersions composed of three components, ciclosporin A (CiA), surfactant (HCO-60) and a pharmaceutical additive, were prepared. As an additive, cellulose acetate phthalate (CAP), methacrylic acid and methacrylic acid methylester copolymer (Eudragit L-100) and hydroxypropylmethylcellulose phthalate (HP-55), which are generally used as enteric coating materials, were employed. The dissolution behavior of CiA from these enteric solid-dispersion system was studied according to the paddle method of JP XI in comparison with that of Sandimmun, an olive oily CiA solution as a reference. Solid dispersion of CiA preparation did not dissolve in the 1st test fluid (pH 1.2) in 2 h. In the 2nd fluid (pH 6.8), about 80% of CiA was dissolved within 12 min, though the dissolution rate was dependent on both the quality and quantity of the additives. An in vivo systemic and lymphatic availability study was performed with rats whose carotid artery and thoracic lymph duct were cannulated. After intrastomach administration of each CiA preparation to rats at a dose of 7 mg/kg, blood and lymph samples were collected for 6 h. One of the HP-55 preparations gave the highest plasma CiA level, Cmax = 0.99 +/- 0.20 (S.E., n = 4) micrograms/ml, and also showed the highest lymphatic availability, the percentage of dose delivered to the lymphatics in 6 h was 1.98 +/- 0.10% and the maximum lymph CiA level was 76.8 +/- 12.86 micrograms/ml. Lymphatic availability of CiA from Sandimmun was 0.78 +/- 0.11% and the peak plasma CiA level was 0.46 +/- 0.10 microgram/ml.(ABSTRACT TRUNCATED AT 250 WORDS)     

The electrochemical behavior of ad-atoms and their effect on hydrogen evolution: Part IV. Tin and lead ad-atoms on platinum

Hydrogen evolution on a platinum electrode decays against X_pt with the deposition of Sn ad-atoms and Pb ad-atoms in the same way as it decays with that of Ge ad-atoms, in which all of these ad-atoms occupy two platinum sites. In general the decay depends on the number of sites occupied by an atom of the ad-atom species.The potential ranges for oxygen adsorption by Sn ad-atoms and Pb ad-atoms are 0.45 to 1.24 V and 0.48 to 0.77 V, respectively, but the oxygen adsorbed by the latter ad-atoms is very small in amount.     

A large thermal hysteresis loop produced by a charge-transfer phase transition in a rubidium manganese hexacyanoferrate

In a rubidium manganese hexacyanoferrate, RbMn[Fe(CN)(6)], the magnetic susceptibility (chi(M)) decreased at 225 K (=T(1/2)decreasing) and abruptly increased at 300 K (=T(1/2)increasing) in the cooling and warming processes, respectively. X-ray photoelectron spectroscopy and infrared spectroscopy indicated that the high-temperature (HT) and low-temperature (LT) phases were composed of Mn(II)-NC-Fe(III) and Mn(III)-NC-Fe(II), respectively. A structural change from cubic (F43m, a = 10.533 A) to tetragonal (I4m2, a = b = 7.090 A, c = 10.520 A) accompanied the phase transition, and, on the basis of these results, the HT and LT phases were assigned to Mn(II)(t(2g)(3)e(g)(2), (6)A(1g); S = (5)/(2))-NC-Fe(III) (t(2g)(5), (2)T(2g); S = (1)/(2)) and Mn(III)(e(g)(2)b(2g)(1)a(1g)(1), (5)B(1g); S = 2)-NC-Fe(II) (b(2g)(2)e(g)(4), (1)A(1g); S = 0), respectively. This phenomenon is caused by a metal-to-metal charge transfer from Mn(II) to Fe(III) and a Jahn-Teller distortion of the produced Mn(III) ion. The reaction mechanism is discussed, considering the entropy difference between the HT and LT phases.     

Indomethacin sustained-release suppositories containing sugar ester in polyethylene glycol base

Indomethacin (IM) sustained-release suppositories were prepared by the fusion method using sugar ester and polyethylene glycol 4000 (PEG). The suppositories were evaluated by in vitro release testing, X-ray analysis and in vivo absorption testing in rabbits. X-ray analysis showed that IM was amorphous in PEG-base suppositories. In a release test, slow-release was obtained when the sugar ester content of a suppository was 60%. The IM plasma level following the administration of the suppository was well sustained in the absorption test. The main slow-release mechanism is considered to be the release of IM from the matrix composed of sugar ester and PEG, which is represented by the Higuchi equation. A good correlation between the release test and the absorption test was obtained. It is considered that the amorphous state of IM in this type of sustained-release suppository would enhance the release and absorption of IM in the rectum of the rabbit, whose rectal fluid volume is small.     

A racemization test in peptide synthesis using 4-(4,6-dimethoxy-1,3,5-triazin-2-yl)-4-methylmorpholinium chloride (DMT-MM)

Racemization of the C-terminal amino acid (Ala) has been studied in various solvents during coupling between 4-methoxybenzyloxycarbonyl (Z(OMe))-Gly-L-Ala-OH and phenylalanine benzyl ester (H-Phe-OBzl) with 4-(4,6-dimethoxy-1,3,5-thiazin-2-yl)-4-methylmorpholinium chloride (DMT-MM). The reaction occurred without substantial racemization in AcOEt, tetrahydrofuran (THF), N,N-dimethylformamide (DMF), CH3CN, and 2-PrOH, while a slight racemization was observed in dimethyl sulfoxide (DMSO), EtOH, and MeOH. The extent of racemization may correlate with the polarity of the solvents.     

Direct UHV-TEM observation of palladium clusters on a silicon surface.

About 1 monolayer of palladium was deposited onto a silicon (111) 7 x 7 surface at a temperature of about 550 K inside an ultrahigh vacuum transmission electron microscope, resulting in formation of Pd2Si nanoislands and a 1 x 1 surface layer. Pd clusters created from an excess of Pd atoms on the 1 x 1 surface layer were directly observed by in situ plan view high-resolution transmission electron microscopy. When an objective aperture was introduced so that electron diffractions less than 0.20 nm were filtered out, the lattice structure of the 1 x 1 surface with 0.33 nm spacing and the Pd clusters with a trimer shape were visualized. It was found that image contrast of the 1 x 1 lattice on the specific height terraces disappeared, and thereby an atomic structure of the Pd clusters was clearly observed. The appearance and disappearance of the 1 x 1 lattice was explained by the effect of the kinematical diffraction. It was identified that a Pd cluster was composed of three Pd atoms without a centered Si atom, which is consistent with the model proposed previously. The feature of the Pd clusters stuck at the surface step was also described.