Nitrogen hydrides safety

In the reaction flask, lithium aluminum hydride (14.4 g, 38 mmol) and benzyltriethylammonium chloride (2.9 g, 13 mmol) are dispersed in tetralin (450 mL) with stirring imder nitrogen. The product of Step 4 (63 mmol of (BrSiH2)4C and toluene) is added dropwise with stirring. The mixture is stirred for 70 h at room temperature, followed by 5 h at 60°C. Toluene and tetra(silyl)methane are then condensed out of the reaction mixture kept at 60°C in a vacuum and collected in a trap held at 10°C. (Small amounts of silane are trapped in a small final trap at -196°C. From there it is allowed to escape through a safety valve to burn upon careful warming of the trap.) The liquid is subjected to fractional distillation and the product collected at 89.5°C, 4.3 g yield (50%). It solidifies in the receiver as colorless cubic crystals, mp 38°C. NMR (benzene-de) 3.84 (s, SiHs) -39.0 (t dez), J(SiC) 31.3, J(CSiH) 5.5) Si -47.8 (q dez), J(SiH) 205.7, J(SiCSiH) 4.6). MS 137-124 (CSi4HJ. 

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