Notes 765 pentachloride. A violent reaction took place. The resulting mixture was kept at room temperature for one hour. Water was then added (100 cc.), the two layers were separated, and the chloroform layer removed to the steambath. During the evaporation of the chloroform the chloride crystallized. It was filtered and dissolved in ether. The ether solution was washed with sodium hydroxide to remove acidic esters. The ether residue after one crystallization gave an almost pure chloride; yield 0.76 g.; m. p. 153°. The mother liquor was evaporated and the residue was distilled in high vacuum and recrystallized from methyl alcohol; yield 0.12 g.; total yield 0.88 g. (83%). Further repeated recrystallizations did not raise the melting point above 154°( uncorr.); [<*]22d + 14.6°( 19.2 mg. in 2 cc. of chloroform solution gave «22d +0.14°, 1-dm. tube).Summary.-A simple method is described for the preparation of dehydroandrosteryl chloride in good yield. The chloro ketone so prepared melts at 154°and has a specific rotation [o:]22d +14.6°.
Methods are described for the use of neocuproine (2,9-dimethyl-l,10-phenanthroline) in determining copper in aluminum and lead-tin solders. The methods are rapid and require no chemical separations except for the extraction of the copper complex, and the results compare favorably with other, more tedious, methods for determining copper. Although the procedure for determining copper in aluminum has been particularly useful for the analysis of high-purity aluminum (99.6 to 99.99% aluminum), it has been applied to high-silicon
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