反应详情

A mixture of 7-formyl-6-(7-hydroxyheptyl)-1,4-dioxaspiro[4,4]nonane (3.88 g.) and 2-methylhexanoyl-methylenetriphenylphosphorane (6.0 g.) in dry tetrahydrofuran (30 ml.) was heated to reflux under nitrogen for 18 hours. The solvent was removed in vacuo and the residue triturated with petroleum ether (b.p. 60°-80° C.), allowed to stand at 0° C., filtered to remove triphenylphosphine oxide and the filtrate evaporated to give 6-(7-hydroxyheptyl)-7-(4-methyl-3-oxooct-1-enyl)-1,4-dioxaspiro[4,4]nonane (5.56 g), νmax 1620 cm-1, 1660 cm-1.

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