Inorganic Synthesis, Vol. 17 by Macdiarmid Alan G.

By Macdiarmid Alan G.

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C. , 1972. G. Zweifel and H. C. Brown, op. , Chap. 1. Submitted by PHILIP C. KELLER’ Checked by HOWARD D. JOHNSON, IIt Bis(dimethy1amino)borane may be prepared by the reduction of CIB[N(CH,),],’ or by gas-phase exchange of hydride and dimethylamino groups on The latter method, using diborane(6) and excess B[N(CH,),], and described here, is the most convenient for the synthesis of a few millimoles of product. The basic vacuum-line techniques necessary to carry out this synthesis are detailed in reference 4.

DIETHYLAMIN0)DIHYDROIDALUMINUM Procedure An apparatus consisting of a 250-mL side-arm Schlenk flask fitted with a Claisen head to which are attached a 50-mL pressure-equalizing dropping funnel and a water condenser is assembled. The water condenser is connected to a mercury-filled bubbler by means of a hose connector. The addition funnel is fitted with a T-type hose connector one arm of which is fitted with a septum and the other arm of which is attached to a source of dry nitrogen and/or a vacuum.

E. J. Corey and R. K. , 93, 7319 (1971). C. A. , 95, 4100 (1973). For stereoselective reductions by other complex borohydrides see: C. A. Brown, S . Krishnamurthy, and S. C. Kim, Chem. , 1973,391; J. Hooz, S . Akiyama, F. J. Cedar, M. J. Benneit, and R. M. Tuggle, J. Amer. Chem. , 96, 274 (1974); also references. G. Zweifel and H. C. Brown, Organic Reactions, 13, 28 (1963). H. C. Brown, “Organic Synthesis via Boranes,” John Wiley & Sons, New York, 1975. D. F. Shriver, “The Manipulation of Air-Sensitive Compounds,” McGraw-Hill Book Company, New York, 1969; also see reference 9 above, pp.

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