The use of HSiMe2OSiMe2H (1) and various hydrodisilanes, R3SiSiMe2H (2; R= alkyl, aryl), as reductants for N, N-dimethylformamide (DMF) in the presence of (Me3N) Mo (CO) 5 as a catalyst led to the formation of a series of novel and structurally interesting siloxanes as well as trimethylamine. In the case of 1 the cyclic poly (dimethylsiloxanes) D 4 and D 6 are obtained, and for 2 the products are bis (disilyl) ethers,(R3SiSiMe2) 2O. ...