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Tetraethylene glycol (TEG) or polyethylene glycol 200 (PEG200) was reacted with CH2Br2 in a modified Williamson synthesis to form oxymethylene‐linked chains. Analytical and preparative gel permeation chromatography plus nuclear magnetic resonance spectroscopy were used to show that the product of reaction consisted of rings with degree of condensation n = 1−15 or more (i.e. 14 to 210 or more atoms in the rings formed from TEG) and chains with molecular weights up to 106 and a wide molecular weight distribution.