Bis trimethylsilyl arsenide

The reaction flask consists of a 100-mL round-bottomed flask blank attached to a 250-mL round-bottomed flask through a Teflon valve. The 250-mL flask has a 24/40 ground glass joint and a gas inlet equipped with a Teflon valve. 

Lithium bis(trimethylsilyl)arsenide is a white powder which is stable at room temperature under an inert atmosphere. It is important for stoichiometric reasons to ascertain whether there is any residual THF. This can be readily determined by H NMR spectroscopy. The H NMR spectrum in C6D6 (reference S 7.15) consists of a single resonance at 0.62. Solubility very soluble in THF and diethyl ether, and minimally soluble in nonethereal solvents. 

Shriver, The Manipulation of Air-Sensitive Compounds, McGraw-Hill, New York, 1969. 

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The reaction of the lithium bis(trimethylsilyl)arsenide (47) with -butyl phosphaethyne (45) <89TH 423-01,93PS(77)45,94JOM(480)45> or a phosphaalkene precursor thereof (46) leads to a mixture of lithium 1,2,4-triphospholide, 1,2,4-diphosphaarsolide (48) and 1,4,2-diphosphaarsolide (49) (Scheme 11). 

TRIS(TRIMETHYLSILYL)ARSINE AND LITHIUM BIS(TRIMETHYLSILYL)ARSENIDE... 

Tris(trimethylsilyl)arsine and lithium bis(trimethylsilyl)arsenide are valuable reagents for dehalosilylation and salt elimination reactions, respectively. Each compound reacts with a wide variety of metal halides to form metal-arsenic bonds.1, 2 The syntheses reported herein are a modification of the published procedures of Becker et al.,3 designed to minimize the use of Schlenk techniques and to allow researchers to prepare two very useful compounds with a minimum of danger. However, since these compounds do... 

Caution. Lithium bis(trimethylsilyl)arsenide is very sensitive to moisture and can react explosively upon exposure to air. Methyllithium is corrosive and reacts violently with water. Both compounds should be manipulated in a dry argon or nitrogen atmosphere. Lithium bis (trimethylsilyl) arsenide should not be heated above 80°C as it begins to decompose. 

The reaction of lithium bis(trimethylsilyl)arsenide 16 with the phosphaalkyne 17 yields an approximately equimolar mixture of lithium 1,2,4- and 1,4,2-diphosphaarsolide 18 and 19 as has been reported in CHEC-II <1994JOM45, 19950M4382, 1996CHEC-II(4)819>. Alkylation of this mixture with bis(trimethylsilyl)bromomethane in DME gives exclusively the 177-1,2,4- and 1 //-l, 4,2-diphosphaarsolcs 20 and 21 (Scheme 3). The two isomers could not... 

Fig. 5. Molecular structures of dimeric zinc bis[bis(trimethylsilyl)arsenide] (left) and trimcric methyl zinc bis(tri-methylsilyl)arsenide (right).

Bis(trimethylsilyl)arsine reacts with diethyl- or dimethylzinc to form different arsenide complexes with the structure dependent on the steric demands of the alkyl group. In the presence of both methyl and ethyl groups alkylzinc bis(trimethylsilylarsenide) forms which has a trimeric solid state structure (37) with a six-membered Zn3As3 and Zn-As distances with an average of 2.48 A.322... 

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