Tris trimethylsilyl arsine

In an inert-atmosphere glove box under an argon atmosphere, the 200-mL upper bulb is charged with 20 g of sodium-potassium alloy (44% 56%)5 

The solution is allowed to cool to room temperature, then the flask is placed in an ice water bath. The stir rate is increased and chlorotrimethylsilane1 is added over a 1.5-h period while adding ice to the water bath to maintain a temperature of 22°C. Upon nearing complete addition of the chlorotrimethylsilane, the solution becomes extremely viscous and the color changes from black to pale gray. The mixture is heated at reflux and stirred vigorously for 24 h. 

1 Aldrich Chemical Company, Inc., 1001 West Saint Paul Avenue, Milwaukee, WI 53233. 

Tris(trimethylsilyl)arsine is a colorless liquid which melts slightly below room temperature, and is stable at room temperature under an inert atmosphere or in a degassed, flame-sealed ampoule. The H NMR spectrum in C7Ds (reference 6 2.09) consists of a single resonance at 5 0.30 and the 13C NMR spectrum shows a single peak at 6 4.31. Solubility very soluble in benzene, toluene, pentane, THF, and diethyl ether. 

Atomergic Chemmetals Corp., 222 Sherwood Avenue, Farmingdale, NY 11735. 

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The reaction of toluene solutions of indium trichloride and tris(trimethylsilyl)arsine resulted in the formation of a very fine dark-brown powder subsequently annealed up to 400°C to drive to completion the elimination of trimethyl-silyl-chloride. Nanocrystalline InAs was obtained. Similar reactions with InBr3 and Inl3 and P compounds have been discussed. Previously a similar reaction was described by Uchida et al. (1993) (reaction of indium acetylacetonate with tris(trimethylsilyl)arsine in refluxing triglyme). Subsequently the reaction with InCl3 was used by Guzelian et al. (1996) in the preparation of nano-crystal quantum dots. They compared different preparation methods and techniques useful to isolate specific size distributions. 

A simUar phosphamethin-cyanine synthesis starting from tris-trimethylsilyl-phosphine has been described by Markl. Using this procedure, arsamethin-cyanines can also be prepared from tris-trimethylsilyl-arsin... 

Tris(trimethylsilyl)arsine is a convenient starting material for the production of LiAs(SiMe3)2-2L (L = coordinating solvent) see, for example, equation (2) and structure (2). 

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. The residues on the glassware and the frit may contain sodium-potassium alloy and/or tris(trimethylsilyl)arsine and should not be exposed to air until disposal. tert-Butyl alcohol and isopropyl alcohol can be used to destroy these pyrophoric compounds however, this should be performed in a fume hood, as arsine gas may be generated. The solid on the frit can be mixed with class D metal fire extinguisher and subsequently treated with either of the aforementioned alcohols. 

The synthetic approach is very similar to the synthesis of 1,3-azaphosphinines <87TL1093>. 1,3-Oxazinium salts (103) react in refluxing acetonitrile with tris(trimethylsilyl)arsine <80ZAAC(462)ll3> by an oxygen-arsenic exchange reaction, to give the 1,3-azarsinines (104) (Equation (20)), which can be isolated as crystalline, fairly stable compounds <88TL535>. 

Harris and co-workers reported the synthesis of cadmium arsenide (Cd3As2) QDs by the fast injection of tris(trimethylsilyl)arsine [(TMS)3As] in TOP into the solution containing cadmium (11) myristate and ODE at 175 °C, which initiated the formation of small particles ca. 2nm) of Cd3As2- The reaction was kept at 175 °C for 20 minutes, which was followed by the secondary slow addition of [(TMS)3As] to produce Cd3As2 QDs of sizes up to 5 nm. The as-obtained QDs were luminescent over a wide spectral range from 530 to 2000 nm, currently the widest range known for a single nanomaterial (Fig. 13). 

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