New bis-crown ethers containing siloxane chain were synthesized. 1,3-Bis(trimethylsiloxy)-1,3-dimethyl-1,3-dipentaoxacyclohexadecamethyl disiloxane (1) was synthesized by reaction of 3-methylene-16-crown-5 (8) with 1,3-bis(trimethylsiloxy)-1,3-dimethyl disiloxane (10) in the presence of Pt catalyst. 1,1,3,3,5,5-Hexamethyl-1,5-dipentaoxacyclohexadecamethyl trisiloxane (2) was synthesized by the reaction of crown ether (8) with 1,1,3,3,5,5-hexamethyl trisiloxane (11) in the presence of Pt catalyst. 3-Methylene-13-crown-4 (7), 3-methylene-16-crown-5 (8), and 3-methylene-19-crown-6 (9) were synthesized by the reaction of triethylene glycol (3), tetraethylene glycol (4), and pentaethylene glycol (5) respectively with 3-chloro-2-chloro-methyl-1-propene (6) in the presence of NaH.