反应详情

A solution containing 119.0 g of non-8-en-2-one, (prepared in Example 22 B-3), 1.2 g p-toluenesulfonic acid monohydrate, 63.1 g of ethylene glycol and 420 ml anhydrous benzene was prepared and refluxed for about 15 to 17 hr. Water which formed was collected in a Dean-Stark trap. The solution was cooled to room temperature and 250 ml of 5% aqueous sodium bicarbonate solution was added thereto. The benzene layer was separated and dried over anhydrous magnesium sulfate and evaporated in vacuo. The residue was distilled to yield 116.8 g of title compound having the following physical characteristics:

1. customwas prepared
2. temperaturerefluxed for about 15 to 17 hr
3. customwas collected in a Dean-Stark trap
4. addition250 ml of 5% aqueous sodium bicarbonate solution was added
5. customThe benzene layer was separated
6. dry with materialdried over anhydrous magnesium sulfate
7. customevaporated in vacuo
8. distillationThe residue was distilled