6-(substituted phenyl)-5-methyl-4,5-dihydro-pyridazin-3(2H)-ones of medicinal interest. The synthesis of SK&F 94836 and SK&F 95654

Two synthetic routes to the dihydropyridazinone-cyanoguanidine 4 (SK&F 94836) are described, both proceeding via the anilino compound 6. An efficient synthesis of the dihydropyridazinone-pyridone 5 (SK&F 95654) is reported. This synthesis proceeds via the fluoro-keto-acid 24 , with subsequent displacement of the fluoro substituent by 4-pyridone. The surprising effectiveness of water as a solvent in this reaction has been highlighted.     

Novel dissolution procedure using a mixture of manganese dioxide and hydrochloric acid for the matrix-independent determination of gold

 A mixture of manganese dioxide and hydrochloric acid has been used for the accurate and precise determination of gold in various gold-bearing matrices. Results of intermethod comparison studies, F-test on variances, Mann-Whitney U-test, Spearman rank correlation and regression analyses are presented. The recommended method can be applied to a quality control programme and for the evaluation of reference materials. Various standard reference materials (SRM) of diverse matrices have been examined to check the validity of the method and the results were found to be in very good agreement with the certified data. Sample decomposition is straight forward [1–10 g sample (roasted at 600–700 °C)+5 g of MnO₂+30 mL of 2 mol/L HCl]. Gold is coprecipitated with potassium tellurite using tin (II) chloride solution. The precipitate is extracted into toluene and finally stripped back into aqua-regia solution for final nebulization into an air-acetylene flame for atomic absorption spectrophotometry. The method is very simple and easily adaptable, and more convenient than conventional methods involving aqua regia or a hydrobromic acid-bromine water mixture. Received: 23 October 1995/Revised: 18 March 1996/Accepted: 23 March 1996     

The effect of ultrasound on the solvolysis of 2-chloro-2-methylpropane in aqueous ethanol

Ultrasonic irradiation has been found to accelerate the solvolysis of 2-chloro-2-methylpropane in aqueous ethanol mixtures from 20 to 60% w/w in ethanol at temperatures between 10° and 25°. The effects are more marked at lower temperatures and higher alcohol compositions with a 20 fold rate acceleration occurring at 10° and 60% w/w. The results also lend independent support to two previous observations that (a) the position of maximum in solvent structuredness is 50% w/w and (b) a logarithmic relationship exists between solvent vapour pressure and ultrasonically enhanced rate constant. At solvent compositions of 50 and 60% w/w ethanol the absolute rate of reaction under irradiation increases with decreasing reaction temperature below 20°.