To a solution of 3 mols butylmagnesiumbromide in ether was added dropwise an one mol of β-cyanoethyloxide. The mixture was refluxed for 1 hour. Then after cooling to the mixture was added hydrochloric acid. An organic layer was dried under sodium sulfate and evaporated. An oil layer was distilled in vacuum. The oxo-3-butane oxide has a boiling point 123-125°C at 15 mm.
A mixture of 100 g of oxo-3-butane oxide, 500 ml ethanol and 15 g Nickel Reney was loaded in autoclave and heated at 45-50°C. In autoclave was introduced a hydrogene. After cooling the mixture was filtered and ethanol was distilled off. 1,1'-Dimethyl-3,3'-oxydipropanol was distilled at 160161°C/18 mm.
