By Macdiarmid Alan G.
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Extra resources for Inorganic Synthesis, Vol. 17
Akad. Nauk SSSR, Ser. , 2830 (1971). 3. D. A. Phillips, Diss. Abstr. D. thesis, University of Washington, Seattle, 1966. 4. R. K. Hertz, H. D. Johnson, 11, and S. G. Shore, Inorg. , 12,1875 (1973). 5. H. Noth and M. Ehemann, Chem. , 1967, 685. 6. D. F. Shriver, “The Manipulation of Air-sensitive Compounds,” McGraw-Hill Book Company, New York, 1969. 7. R. T. , New York, 1948. 8. W. L. Jolly, “The Synthesis and Characterization of Inorganic Compounds,” Chap. , 1970. 7. POTASSIUM TRI(sec-BUTYL)HYDROBORATE(l-) (sec-C4H,),B + KH(s) 2% K+[(sec-C,H,),BH]- Submitted by CHARLES ALLAN BROWN* Checked by SHELDON C.
The mass spectrum shows only peaks characteristic of the monomer (parent ion m/e 57) when a heated inlet system is used; if all inlet heaters are turned off, the spectrum shows an envelope of peaks characteristic of the dimer (parent ion m/e 114). 3 References 1. E. Wiberg, A. Bolz, and P. Buchheit, Z. Anorg. , 256, 285 (1948). 2. G. W. Schaeffer and E. R. Anderson, J. Amer. Chem. , 71,2143 (1949). 3. A. B. Burg and C. L. , ibid, 71, 3451 (1949). 4. V. R. Miller and G. E. , 92, 1558 (1970). 34 Inorganic Syntheses 5.
Disposal of the pentane washes should be carried out with the precautions previously described for excess potassium hydride. Potassium Tri(seebuty1)hydroborate (1-) 29 6 mL of THF and 2 mL of water, under inert gas. 5 mL of 3N aqueous sodium or potassium hydroxide solution. 5 mL of 30% hydrogen peroxide is added over 15-30 min. (B Caution. ) After all the hydrogen peroxide is added, the solution is heated for 10 min at 50°, cooled to room temperature, and treated with crystalline potassium carbonate to produce a saturated lower aqueous layer and a clear upper THF layer.