By John J. Eisch
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Additional resources for Organometallic Syntheses. Nontransition-Metal Compounds
Eng. Chem. Anal. Ed. 18, 5 2 (1946)] recommend the passge of a peroxide-containing solvent through a column of activated alumina. Of great advantage is that the eluate is at once free of peroxides and is essentially anhydrous. See G. Wohlleben [Angew. Chem. 67, 741 (1955)] for the drying of solvents with activated alumina. 26 A. Anhydrous and Anaerobic Reaction Media of the purified solvent is injected into the apparatus. Then via an inserted syringe a solution of lithium aluminum hydride in dry T H F is added d r o p wise.
See G. Bahr and G. Muller, Chem. Ber. 88, 251 (1955). H. Schlesinger and H. Brown, J. Am. Chem. Soc. 62, 3433 (1940). 5. Storage and Transfer of Organometallic Compounds 37 FIG. 20. Technique for filling ampuls with liquid organometallics. A , Movable hollow glass tube bearing a wire support (D) for inverted glass ampuls ( E ) ; B, rubber tubing for a snug, flexible contact; C , adapter whose upper tube fits A closely; F , liquid to be sampled; G , when immersed, ampul should be just below the surface; H, inert gas source; I, three-way stopcock; J, vacuum.
Lehmkuhl, W. Pfohl, and K. Zosel, Justus Liebigs Ann. Chem. 629, 1 (1960). F. J. Radd and W. W. S. Patent 3,104,252 (September 17, 1963) [Chem. Abstr. 60, 547 (1964)]. C. W. Kamienski and D. L. Esmay, J. Org. Chem. 25, 1807 (1960). W. S. Johnson and G. H. Daub, in "Organic Reactions" (R. ), Vol. VI, pp. 42-44, Wiley, New York, 1951. D. T. Hurd and E. G. Rochow, J. Am. Chem. Soc. 67, 1057 (1945). C. R. Noller, in "Organic Syntheses" (A. H. ), Coll. Vol. II, p. 184. Wiley, New York, 1943. H. Gilman and E.