Relationship between formation conditions, properties, and crystallite size of boehmite

Boehmites (gamma-AlOOH) with a variety of crystallite sizes were prepared under various precipitation conditions from solutions of aluminum nitrate and sodium aluminate and also by hydrothermal treatment of a commercial boehmite powder. The relationships between the crystallite size and other properties of the boehmites were investigated. Crystalline boehmite was formed in the pH range 7 to 10 while gels precipitated below pH 7 and bayerite (Al(OH)3) formed at pH 11. The crystallite size of the boehmite increased at higher pH, higher temperature of the precursor solution, and longer aging time. As the crystallite size of the boehmite increased, the specific surface area, pore volume, and excess water decreased. Boehmites of small crystallite size, called pseudoboehmite, showed broadened X-ray peak widths and increased d-spacing of the 020 reflection. These changes are attributed to the small crystallite size (smaller numbers of stacking layers) and also to excess water in the interlayers of the boehmite structure.     

Stereoselective synthesis of spirocyclic oxindoles based on a one-pot Ullmann coupling/Claisen rearrangement and its application to the synthesis of a hexahydropyrrolo[2,3-b]indole alkaloid

An efficient and convenient approach to the synthesis of spirocyclic oxindoles from iodoindoles has been developed. The most striking feature of this approach is that the sequential intramolecular Ullmann coupling and Claisen rearrangement proceeds in a one-pot manner to afford 3-spiro-2-oxindoles in good yield with excellent diastereoselectivity. Application of this one-pot reaction to chiral non-racemic tertiary alcohol substrates resulted in complete chirality transfer to the spirocyclic quaternary carbon. Using this method, asymmetric total synthesis of (−)-debromoflustramine B was accomplished.     

A new spectroscopic method using the Fraunhofer diffraction pattern

Conclusions From the results shown above, it may be said that this new spectroscopic method using the Fraunhofer diffraction pattern has the possibility of practical use. This method has the advantages that the multiplex gain is retained and the experimental apparatus is very simple as compared with the conventional grating spectroscopy. The resolution is about 1.25A/2KX and becomes higher with the increase of the number of slits and the maximum value of variable in the diffraction pattern. The other way, the simultaneous equations become more difficult to solve with the increase of resolution and at present the maximum value of N_S is 21. In such a case the adjustment factor A and the figure of condition of matrix are important. Further, large memory of the electronic computer is required, for example, 2.56MB for N=800. The experimental setup is now under construction in order to verify the usefulness of this method in the far infrared region.     

Shear-Force Detection by Reusable Quartz Tuning Fork without External Vibration

Many studies have reported on the use of quartz tuning forks (a type of crystal oscillator used in wristwatches) in the detection of shear force, employed to control the distance between the probe and the sample in a scanning near-field optical microscope. This study focuses on a newly-devised shear force detection method capable of simultaneous non-external oscillation and detection, which also allows for subsequent reuse of a tuning fork. The optimum configuration and tip length for inserting a probe into the slit of a tuning fork have been elucidated. The shear force was detectable in about 5 nm decay length using such conditions.     

Characteristics of the Na/beta-alumina/Na cell as a sodium vapor pressure sensor

The EMF and voltage-current characteristics for a galvanic cell with the configuration Na vapor (P₁)/sodium beta-alumina/Na vapor (P₂) were studied. It was verified that the EMF followed the Nernst relation over a wide pressure range. For example, when P₁ = 2 × 10^-2 mm Hg and beta-alumina temperature = 340°C, the measured EMF agreed with the calculated value in P₂ range from 10^-5 to 10^-2 mm Hg. At lower pressure range, the measured EMF showed a negative deviation. Coexisting argon gas did not influence the cell EMF characteristic. In an atmosphere containing oxygen, the measured EMF was very high at first. Then it decreased and finally approached a value which agreed with the Nernst equation after several hours. At low beta-alumina temperatures, current saturation was observed in the voltage versus current relation with the anode on the P₂ side. Although the sodium pressure could be determined from saturating current measurement, the measurable pressure range was narrower than that for EMF measurement. At high beta-alumina temperature, current saturation was not clear. Values of 6 × 10^-6 (Ω cm)^-1 for the electron conductivity and 6 × 10^-10 (Ω cm)^-1 for the hole conductivity at 340° were obtained for beta-alumina from the voltage-current characteristics at low sodium pressure.     

Total synthesis of (+/-)-gleenol and (+/-)-axenol via a functionalized spiro[4.5]decane

Total synthesis of the biologically important axane sesquiterpenes, gleenol (1) and axenol (2), was accomplished through a readily available spiro[4.5]decane. The key features of the synthesis of 1 and 2 include Claisen rearrangement to afford the multi-functionalized spiro[4.5]decane 4 as a single diastereomer in excellent yield, installation of the C7 isopropyl group via ketene dithioacetal instead of direct alkylation and a diastereoselective reduction of ketone under the Birch conditions.     

Synthetic study on telomerase inhibitor, D8646-2-6: synthesis of the key intermediate using Sn(OTf)2 or Sc(OTf)3 mediated aldol-type reaction and Stille coupling

The synthesis of the key intermediate (4) in the proposed route to D8646-2-6 is described. The aldol reaction of the carbohydrate-containing pyrone 7 with the aldehyde 6 was accomplished by using LiHMDS and Sc(OTf)3 or Sn(OTf)2. The stepwise dehydration reaction of the aldol adduct 14, followed by Stille coupling with vinyl stannane 5 which contained phosphonate gave the desired 4.     

N-fused carbazole-zinc porphyrin-free-base porphyrin triad for efficient near-IR dye-sensitized solar cells

N-fused carbazole-zinc porphyrin-free-base porphyrin triad featuring an ethynyl-linkage was synthesized; efficient sensitization as long as 900 nm was demonstrated and an overall light-to-electricity conversion efficiency of 5.21% was achieved under AM 1.5 G one sun illumination.