Porous plate, acid-washed kaolin, activated alumina, pumice, aluminum, and iron were employed as carriers for vanadium pentoxide with some success. Molybdenum oxide on porous plate and vanadium pentoxide-molybdenum oxide (1 to 1) mixture on acid-treated pumice had some catalytic action. Traces of nitrile were detected when the following were employed as catalysts: silver vanadate on acid-washed porous plate, vanadium pentoxide on iron, platinized aerogel, alkali-washed kaolin, vanadium pentoxide-thorium oxide (3 to 2), titanium dioxide on kaolin, and cupric oxide or potassium bisulfate on acid-washed pumice.The activity of the fused vanadium pentoxide was retained over an extended period of use. In experiment 38 a 31.7% yield of nitrile was obtained after the catalyst had been used for 13 hours. After 97 hours a 33.1% yield of nicotinonitrile was obtained in experiment 39 under experimental conditions otherwise comparable to those of experiment 38.
ACKNOWLEDGMENTThe authors are indebted to C. O. Willits and W. L. Porter of the Analytical and Physical Chemistry Division for the analyses upon which the yields of nicotinonitrile were based.
LITERATURE CITED(1) Graver (to Barrett Co.), U. S.
Notes 49 sulfide was complete. After filtration, the filtrate was evaporated in vacuo to yield a yellow sirup which was used directly for the next step in the synthesis.In another similar preparation, the sirup was treated with absolute alcohol and anhydrous ether and allowed to crystallize in an icebox. The small amount of crystalline material separating was recrystallized from re-butanolether, needles m. p. 134°dec. Due to the unstable nature of (II), satisfactory analytical figures were not obtained.2-Mercapto-4(5) -methyl-5(4)-(/3-hydroxyethyl) -imidazole ( )* was obtained in good yield from the unstable crystalline (II).' More conveniently it was prepared as follows: The crude sirup resulting from the reduction of 14 g. of (I) was taken up in 50 cc. of ethanol, 10 g. of
Two cases exhibiting the Mobitz-type of second-degree atrioventricular heart block are reported.
This rhythm may be unstable, and progression to complete heart block and Adams-Stokes seizures has been observed.
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