By Wold A. (ed.), Ruff J.K. (ed.)
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Additional resources for Inorganic Synthesis, Vol. 14
The lamp is turned on only after the Vycor *Fischer and Porter Company, Warminster, Pa. 18974. +Air Products and Chemicals, Box 558, Allentown, Pa. 18100. , Newark, N J. 07100. Otlorodijluorwmine and Difluorodkzene 37 n Fig. 5. Pyrex g&ssphotolysis yessel with water-cooled quartz probe. filter is in place, the cold tap water is passing through the water jacket, and the reagents are at room temperature. Photolysis time for an 850-ml. bulb is about 90 minutes. After the photolysis is completed, the reaction mixture is transferred under dynamic vacuum to a trap at -195°C.
18 Inorgonic Syntheses Ice-acetone condenser, a mechanical stirrer, a nitrogen gas inlet-outlet system, and the pressure-equalizing addition funnel containing the tetramethyldiphosphine. The liquid ammonia is maintained a t -78OC. during the reactions. 37 mole) are added to the liquid ammonia, which produces a blue solution. 1 85 mole) is added dropwise. A deep-green solution develops as the diphosphine is added. The addition funnel is rinsed with 25 ml. 7 g. 18 mole) of 1,3-dichloropropane in 5 0 ml.
31, 1542 (1969). 10. 3(C2H5)20]+ 3LiCI Submitted by D. L. SCHMIDT,*C. B. ROBERTS,* and P. F. REIGLER* O w k e d by M. F. ,? and E. P. 3 [ (C,H5 )2 01 ,$ have been published,'S2 but the absence of complete experimental details makes duplication difficult. ' Problems inherent in previous methods, such as premature precipitation, decomposition of the alane, and lithium chloride contamination, are avoided. ) in the reaction mixture. Purified reactants, as well as minimal exposure to light and higher temperatures, *The Dow Chemical Company, Midland, Mich.
Inorganic Synthesis, Vol. 14 by Wold A. (ed.), Ruff J.K. (ed.)