Disilylmethane is available in a four‐step synthesis starting with phenylsilane. This is converted into chlorophenylsilane by HCl/AlCl3. The reaction of PhSiH2Cl and dibromomethane with magnesium in tetrahydrofuran affords bis(phenylsilyl)‐methane, which yields bis(bromosilyl)methane by treatment with anhydrous hydrogen bromide. (BrH2Si)2CH2 is converted into disilylmethane by reduction with LiAlH4 in a two‐phase system using a phase‐transfer catalyst. ‐ Methyldisilane is available by alkylation of a monohalodisilane, XSi2H5 (X  Cl, Br), with methyllithium in a high‐boiling ether or by silylation of bromomethylsilane with silylpotassium. Due to secondary silylation reactions the overall yields of methyldisilane are low in all cases.

As a precursor for trisilylmethane, tris(phenylsilyl)methane is prepared by a Merker‐Scott reaction of chlorophenylsilane, bromoform, and magnesium turnings in boiling tetrahydrofuran. Chlorophenylsilane is formed in a new synthesis starting from phenylsilane and hydrogen choride/AlCl3 in diethyl ether. The gas phase structure of trisilylmethane (H3Si)3CH, obtained from (PhSiH2)3CH via (BrSiH2)3CH, has been determined by electron diffraction. Data refinement confirmed a model of C3 molecular symmetry, with local C3v symmetry for the silyl groups. — As a precursor for 1,1,1‐trisilylethane, 1,1,1‐tris(phenylsilyl)ethane has been prepared similarly from chlorophenylsilane, 1,1,1‐trichloroethane and magnesium and converted via 1,1,1‐tris(bromosilyl)ethane into CH3C(SiH3)3.

The residue above, 37-39, and fractions 7-8 were combined and fractionated through column X to give 5.0 g. of methylneopentylcarbinol, »md 1.4175-1.4195, which gave an -naphthylurethan, m. p. and mixed m. p., 86-87°. This was checked with a 3,5-dinitrobenzoate, m. p. and mixed m. p., 95-95.5°. This sample, together with the 6.6 g. of fractions 40-41, represents a 3.4% yield of reduction product. Attempts to find 2-heptanol were unsuccessful. Fractions 9-17 contained dodecenes (0.63 mole) and fractions 18-30 contained methyl-re-amylneopentylcarbinol.

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ChemInform is a weekly Abstracting Service, delivering concise information at a glance that was extracted from about 100 leading journals. To access a ChemInform Abstract of an article which was published elsewhere, please select a “Full Text” option. The original article is trackable via the “References” option.