Synthesis of a C4-epi-C1-C6 fragment of FR901464 using a novel bromolactolization

[reaction: see text] A synthesis of a C4-epi-C1-C6 fragment of the antitumor agent FR901464 is reported. The advanced intermediate prepared in this study contains two of the three correct stereocenters found in the C1-C6 moiety of FR901464. For the preparation of this intermediate, we have developed a highly diastereoselective bromolactolization of a delta-alkenyl ketone.     

Radiocesium concentration in milk after the Chernobyl accident in Japan

Radiocesium concentrations in cow's milk from two producing districts in Japan were measured monthly for three years following the Chernobyl accident. The Chernobyl contribution in¹³⁷Cs concentration was evaluated from the¹³⁴Cs concentration and the¹³⁷Cs/¹³⁴Cs ratio. The highest¹³⁷Cs concentration of 0.6 Bq l^–1 was observed in May 1986 and the Chernobyl contribution has decreased during three years to levels corresponding to the contribution from past nuclear weapons fallout. Annual values of child internal dose through milk consumption were estimated at 0.6, 0.3 and 0.1 Sv for the first, the second and the third year following the accident, respectively.     

Effective UV photolytic decomposition of organic compounds with a low-pressure mercury lamp as pretreatment for voltammetric analysis of trace metals

The effectivity of UV irradiation with low and high pressure mercury (L-Hg and H-Hg) lamps on the decomposition of organic compounds in aqueous solutions, as pretreatment for the voltammetric determination of trace metals, is compared. The photolytic decomposition with the L-Hg lamp was much faster than with the H-Hg lamp. The higher efficiency of the L-Hg lamp is caused by its greater light intensity at short wavelengths. Interferences of organic compounds on the voltammetric determination of nickel and indium were eliminated successfully by 90 min irradiation with the L-Hg lamp. Humic acid and organic interference with the voltammetric determination of nickel in natural river water were successfully eliminated. The decomposition using the L-Hg lamp can be carried out without added oxidizing reagents and at room temperature, thus eliminating loss of water samples by evaporation at higher temperature.     

Isolation of the complex between acrylonitrile and trimethylaluminum

The complex of acrylonitrile (AN) with trimethylaluminum (AlMe₃) was successfully isolated as a white needlelike crystal with a melting point of 42.5°C. In this article the preparation of the complex is described in detail. Cryoscopic and spectral investigations indicated that the complex is formed by an equimolar ratio of AN and AlMe₃. From the measurement of the x-ray diffraction photograph of the crystal the repeat period was determined to be 9.47 ± 0.05 Å.     

Studies toward an ideal fluorescence method to measure palladium in functionalized organic molecules: effects of sodium borohydride, temperature, phosphine ligand, and phosphate ions on kinetics

Residual metals in fine chemicals are currently detected by using inductively coupled plasma mass spectrometry, which requires expensive instrumentation and does not have high-throughput capabilities. Although fluorescent probes can be amenable to high-throughput analyses of metals, the utility of such analyses is limited due to the lack of generality. Herein, we report a significant improvement (≈19-fold) to our previously reported catalysis-based fluorescent probe for palladium. Specifically, we found that slightly elevated temperature dramatically improved the generality of the method and that the deallylation reaction of the nonfluorescent compound 1 was accelerated by phosphate ions in aqueous media. This method was capable of detecting 0.2 ppb palladium. We demonstrated reasonably accurate palladium detection in various active pharmaceutical ingredients and highly functionalized organic compounds.     

Simultaneous two-photon excited fluorescence and one-photon excited phosphorescence from single molecules of an organometallic complex Ir(ppy)3

We report a study of excited-state lifetimes of the phosphorescent organometallic complex Ir(ppy)3 on ensemble and a single-molecule level. With decreasing concentration, an increasingly intense fast component of 3 ns lifetime appears next to the 1.1 mus phosphorescence. Experimental evidence suggests that strong two-photon absorption followed by fluorescence is responsible for the fast lifetime component.