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With di-isopropyl azodicarboxylate; triphenylphosphine; In tetrahydrofuran; at -10 - 25℃; for 21h;
A solution of 1.4 g (7.36 mmol) of 2-[4-(trifluoromethyl)phenyl]ethanol, 2.22 g (8.47 mmol) of triphenylphosphine and 0.82 g (8.1 mmol) of 1,3-<strong>[2346-26-1]oxazolidine-2,4-dione</strong> (J. Med. Chem. 1991, 34, 1542-1543) in 25 ml of tetrahydrofuran, cooled to approximately -10 C., is admixed dropwise under an inert atmosphere with a solution of 1.7 g (8.47 mmol) of diisopropyl azidocarboxylate (DIAD) in 5 ml of tetrahydrofuran, while maintaining the temperature of the reaction mixture between -10 C. and 0 C. Stirring is continued at 0 C. for 1 hour and then at 25 C. for 20 hours. The filtrate is concentrated under reduced pressure and the residue is taken up in dichloromethane and aqueous 5% sodium hydroxide solution (10 ml). The aqueous phase is separated and then extracted twice with dichloromethane. The organic phases are combined and washed in succession with aqueous hydrochloric acid solution (1N) and then saturated aqueous sodium hydrogencarbonate solution and saturated aqueous sodium chloride solution. The organic phase is dried over sodium sulphate and the filtrate is concentrated under reduced pressure. The residue thus obtained is purified by chromatography on silica gel, eluting with a 20/80 mixture of ethyl acetate and cyclohexane. This gives 1.5 g of oxazolidinedione in the form of an oil
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