By Alan G. Macdiarmid
The volumes during this carrying on with sequence supply a compilation of present ideas and concepts in inorganic artificial chemistry. contains inorganic polymer syntheses and practise of vital inorganic solids, syntheses utilized in the improvement of pharmacologically energetic inorganic compounds, small-molecule coordination complexes, and comparable compounds. additionally includes priceless info on transition organometallic compounds together with species with metal-metal cluster molecules. All syntheses awarded the following were validated.
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Additional info for Inorganic Syntheses, Volume 17
5 mL, 120 mmol) of methyl iodide with stirring. A white precipitate of [P(C6H5),CH,]I begins to form almost immediately. The mixture is stirred for 36 hr. 2 mL, 20 mmol) portion of methyl iodide is added after 12 hr and another portion after 24 hr to replace evaporation losses. Use of an excess of methyl iodide makes recrystallization unnecessary. 7%) Of [P(C6H5),CH3]1. * The column must contain little or no water and should be eluted with absolute ethanol. Care should be taken to ascertain that the column is of sufficient capacity to handle all of the iodide.
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. 202-21 1. H. 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.
24 Inorganic Syntheses Properties Tetrabutylammonium tetrahydroborate( 1- ) is a white, crystalline solid, moderately stable in air at room temperature. It is soluble in methylene chloride, chloroform, methanol, ethanol, water, tetrahydrofuran, and benzene, but insoluble in diethyl ether and pentane. IBH= 82 Hz) characteristic of [BH,)-. The "B nmr spectrum is similar to that of [P(C,H,),CH,][BH,]. C. METHYLTRIPHENYLPHOSPHONIUM HEPTAHYDRODIBORATE(1 -) [P(C6H5)3CH3][BH41 f 3B2H6 - [P(C6H5)3CH31[B2H71 Procedure Caution.
Inorganic Syntheses, Volume 17 by Alan G. Macdiarmid