A general and convenient method for the synthesis of unesterified carbamoyl- and thiocarbamoyl-phosphonic acids

Unesterified carbamoyl- and thiocarbamoyl-phosphonic acids were prepared in high yields by the reaction of tris(trimethylsilyl) phosphite with isocyanates and isothiocyanates followed by treatment of the 1:1 carbonyl adducts with aniline-containing methanol.     

Structural assignment of n3-acylated uridine derivatives by means of 13c nmr spectroscopy

Diisopropylethylamine was effective as a base for acylation of 2′,3′,5′-tri-O-acetyluridine with various acid chlorides. The ¹³C NMR spectra of the products and related compounds showed clearly that the acyl groups intoduced to the uracil moiety are attached to the N³-nitrogen.     

Epithermal neutron diffraction from a gadolinium alloy (Gd0.9Y0.1)

The coherent nuclear scattering amplitude of natural Gd was determined by epithermal neutron diffraction with neutron energy of 1.4 eV to be 1.4 ± 0.1 × 10^?12 cm.     

Automatic extraction using the mini-column liquid chromatography method for analysis of drugs of abuse in biological fluids

Summary The preparation of an automatic extractor using ODS-minicolumn (25mm × 9mm i.d.) for analysis of drugs of abuse in biological fluids and its application are described. The auto-extraction method consists of the sequential operations, adsorption-washing (clean up)-elution(collection of the analyte) and regeneration of column, which continue repeatedly. Recoveries of drugs from spiked plasma and urine samples with the auto-extractor were almost quantitative at the optimum pH and much better than that of the conventional extraction with ether. Reproducibility of the auto-extraction was fairly good and the relative standard deviations of 10 measurements for methamphetamine, THC, morphine, cocaine and methaqualone in urine and plasma were from 0.55% to 4.35%. The simultaneous extractions of methamphetamine, THC, tranquilizers and their metabolites in urine with the autoextractor are presented as applications. Presented at the 15th International Symposium on Chromatography, Nürnberg, October 1984     

Synthesis and hybridization properties of oligodeoxynucleotides incorporating 2-N-carbamoylguanine derivatives as guanine analogs

2-N-Carbamoyldeoxyguanosine and its derivatives were synthesized and incorporated into ODNs. The T_m analyses revealed higher selective base recognition ability of 2-N-carbamoylguanine than that of guanine. The new guanine analog must be useful for the development of functional oligodeoxynucleotides capable of precise base recognition.     

Chemically stabilized phenylboranylidene groups having a dimethoxytrityl group as a colorimetrically detectable protecting group designed for cis-1,2-diol functions of ribonucleosides in the solid-phase synthesis of m2(2,2)G5'ppT

To not only improve the inherently poor stability of the phenylboranylidene group as a protecting group of the 2',3'-cis-diol function of ribonucleosides but also introduce a colorimetrically detectable function into its mother structure, various 2-[(dialkylamino)methyl]phenylboronic acid derivatives having a [(4,4'-dimethoxytrityl)oxy]methyl group were synthesized. The reaction of uridine with these substituted phenylboronic acid derivatives gave the corresponding 2',3'-O-phenylboranylideneuridine derivatives. The stability of these phenylboranylidene groups was examined. As a result, it was shown that the steric hindrance around the amino group greatly influenced the stability of the 2-substituted phenylboranylidene groups. The 2-aminomethyl-5-[[(4,4'-dimethoxytrityl)oxy]methyl]phenylboranylidene group was the most stable. Its 2-dimethylamino counterpart, the 2-[(dimethylamino)methyl]-5-[[(4,4'-dimethoxytrityl)oxy]methyl]phenylboranylidene group, was the second most stable. When the most and second stable protecting groups were applied to the synthesis of m(2)(2,2)G(5)(')ppT on controlled pore glass, the second stable protecting group showed the best result. The use of this DMTr-containing protecting group enabled us to estimate colorimetrically the amount of the m(2)(2,2)G residue that was incorporated into the reactive site of the pT-loaded CPG resin.     

Synthesis and characterization of new nitridotechnetium-EDTA complex

TcN-EDTA has been synthesized for the first time starting from TcNCl₄ ^–. Elemental analysis shows that this compound has three molecules of water of crystallization: TcN(Hedta) · 3H₂O. Its optical spectrum has an absorption maximum at 505 nm with = 1060 dm³.mol^–1.cm^–1. It decomposed easily under alkaline conditions.     

A new approach to the study of normalized appearance energy of hot atom reaction product in optical isomers of tris/acetylacetonato/ruthenium/III/

Appearance energy is originally the threshold energy at which récoil products begin to be observed. This was determined by /, '/ reactions. Afterwards, an alternative technique has been developed to determine it by summing up recoil energy spectrum. The latter technique assumed a step function rising at energy E_O in the yield-energy relation. E_O should be defined as normalized appearance energy /NAE/, because it is not threshold energy in its original sense. The NAE for isomerization from to /or reverse/ in Ru/acac/₃ was estimated to be 29 eV, and that for free atom /or ion/ formation was calculated to be 34 eV. The 5 eV difference seems to indicate an energy interval in which isomerization effectively occurs in the recoil reaction.