Microwave-Assisted Phospha-Michael Reactions with Internal Alkenes

The atom efficient phospha-Michael reaction between bis 4-methylphenyl phosphine oxide and several activated internal alkenes has been shown to occur under microwave irradiation without added solvent or catalyst. The alkenes used for this study were ethyl 4-nitrocinnamate, two chalcones ((E)-3-(4-methoxy-phenyl)-1-(4- nitrophenyl)-prop-2-en-1-one and (E)-1-(4-methoxyphenyl)-3-(3-nitro-phenyl)-prop-2- en-1-one), and 2-phenylmethylene-propanedinitrile. In the case of ethyl 4-nitrocinnamate, reaction with bis 4-methylphenyl phosphine oxide for sixty minutes at 130 °C yielded the desired phospha-Michael product in a 55% yield after purification. Varying the location of the nitro group on the phenyl rings of the chalcones did not seem to have a large effect on their reactivity. By NMR, both chalcones seemed to react to the same extent when the reaction times and temperatures were held constant. Interestingly, a phospha-Michael reaction was observed at a reaction temperature of 65°C for experiments involving 2- phenyl-methylene-propanedinitrile while the other substrates required a reaction temperature of 130 °C. Similar experiments were carried out with bis mesityl phosphine oxide and two internal alkenes: 2-phenylmethylene-propanedinitrile and ethyl-2-cyano-3- methyl-2-butenoate. These experiments did not yield any of the predicted phospha- Michael products, which suggest steric limitations to the Michael donor for this reaction.

Ammoniacal Sulphate Leach of Ananconda Zinc Calcine Recovery of the Zinc by Electrolysis.

Zinc is produced from ores by two general methods, distillation and electrolysis. The general principles involved in the electrolytic zinc process of today were known as far back as 1880. Difficulties encountered in purifying the solution for electrolysis and lack of suitable mechanical apparatus were the main reasons that such a long time elapsed before the process was used to produce zinc in commercial quantities.

Alkali Leaching of Antimony Sulphide and Electrolytic Recovery of Antimony from the Resulting Leach Solution

It is the purpose of this investigation to obtain some insight into optimum conditions for leaching Stib­nite with sodium hydroxide solution and also to steady the factors affecting the electrolysis of the resulting solution.