Sodium Hydroxide → HCID 19887357, compound

Participants

Reaction Steps

20.4 g of 8-[4,4-bis(4-fluorophenyl)-3-butenyl]-3-cyclohexyl-4-hydroxy-4-methyl-2-oxo-1-oxa-3,8-diazaspiro[4,5]decane are boiled with 1.52 g of p-toluenesulfonic acid monohydrate in 204 ml of xylene while stirring in an apparatus fitted with a water-trap and azeotropically distilling off the water formed in the reaction. After the termination of the reaction (about 2 hours) the reaction mixture is cooled down and its pH value is adjusted to 9-10 by adding 5% by weight aqueous sodium hydroxide solution. Then, the organic phase is washed with water to neutral, dried over anhydrous sodium sulfate and evaporated under reduced pressure. After recrystallizing the residue from a mixture of benzene and ethanol, the title product is obtained in 90.3% yield, m.p.: 145°-146° C.

Provenance & Evidence