2-ethyl-1,6-dioxaspiro[4.4]nonane

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 0.540 g of mercury oxide in 100 ml of distilled water and 3.6 ml of concentrated H2SO4 were heated at 60° and at this temperature non-4-yn-1,7-diol (3.0 g) was added to the reaction mixture, which was then left 30 min under stirring. After cooling to room temperature, the mixture was extracted twice with diethyl ether washed with an aqueous solution of NaHCO3 and brine until neutrality, and finally dried over Na2SO4. The volatiles were taken off by evaporation in vacuo and the obtained residue was distilled in a bulb apparatus. 2.3 g (yield 35.2%) of the desired 2-ethyl-1,6-dioxaspiro[4.4]nonane having b.p. 80°-90°/1 Torr were thus obtained. The product had a purity of ca. 97%. was added to the reaction mixture, which the mixture was extracted twice with diethyl ether washed with an aqueous solution of NaHCO3 and brine until neutrality finally dried over Na2SO4 The volatiles were taken off by evaporation in vacuo the obtained residue was distilled in a bulb apparatus