Abstract Four 1, 3-bis (ω-hydroxyalkyl) tetramethyldisiloxanes [HO (CH 2) n SiMe 2] 2 O (I;(n= 3–6) were synthesized by methanolysis of the corresponding trimethylsilyl-terminated disiloxanes (III). The latter were obtained from 1, 1, 3, 3-tetramethyldisiloxane (II) and the appropriate (ω-alkenyloxy) trimethylsilanes (IV). Under acidic conditions III formed in addition to I, the corresponding (ω-hydroxyalkyl) pentamethyldisiloxanes HO (CH 2) n ...