反应详情

A mixture of 7-formyl-6-(7 -hydroxyheptyl)-1,4-dioxaspiro[4,4]nonane (4.2 g.) and propoxyacetylmethylenetriphenylphosphorane (7.18 g.) in dry tetrahydrofuran (35 ml.) was heated at reflux under nitrogen for 18 hours. The solvent was removed in vacuo and the residue triturated with a mixture of petroleum ether (b.p. 60°-80° C.) and ethyl acetate, allowed to stand at 0° C., filtered to remove triphenylphosphine oxide and the filtrate evaporated to dryness to give 6-(7-hydroxyheptyl)- 7-(3-oxo-4 -propoxybut-1-enyl)-1,4-dioxaspiro[4,4]nonane (8.6 g.), νmax 1620 cm-1, 1680 cm-1.

1. temperaturewas heated
2. temperatureat reflux under nitrogen for 18 hours
3. customThe solvent was removed in vacuo
4. customthe residue triturated with a mixture of petroleum ether (b.p. 60°-80° C.) and ethyl acetate
5. customto stand at 0° C.
6. filtrationfiltered
7. customto remove triphenylphosphine oxide
8. customthe filtrate evaporated to dryness