A Synthetic Pathway to 1,3‐Bis(trisilylmethyl)disiloxane [(H3Si)3CSiH2]2O — the Octasila Analogue of Dineopentyl Ether [(H3C)3CCH2]2O

A synthetic route to partly silylated tetra(silyl)methanes (ArH2Si)nC(SiH3)4 — n′ to their precursors (TfH2Si)nC‐(SiH2Ar)4 — n (Ar = p‐tolyl, phenyl; Tf = CF3SO3; n = 3, 2, 1), and to 1,3‐bis(trisilylmethyl)disiloxane [(H3Si)3CSiH2]2O (9) is reported. Starting from symmetrical tetrakis(arylsilyl)‐methanes (aryl = p‐tolyl, phenyl), we have obtained the selectively dearylated (arylsilyl)silylmethanes (ArH2Si)nC(SiH3)4 — n (Ar = p‐tolyl, phenyl; n = 3, 2, 1) by Si—Ar cleavage with equivalent quantities of trifluoromethanesulfonic acid (triflic acid) and hydrogenation of the corresponding silyl triflates (TfH2Si)nC(SiH2Ar)4 — n (n = 3, 2, 1) with LiAlH4. The synthesis of 9 has been accomplished by treating trisilyl(p‐tolylsilyl)methane p‐TolH2SiC(SiH3)3 (7) with stoichiometric amounts of triflic acid to give (trisilylmethyl)silyl triflate TfH2SiC(SiH3)3 (8) and hydrolysing the latter with water.