Mitsunobu反应中醇的旋转

hr. The reaction mixture is cooled to room temperature, diluted with 150 mL of ether, and washedtwice with 100 mL portions of saturated aqueous sodium bicarbonate solution. The aqueous layers arecombined and back-extracted with 100 mL of ether. The combined organic layers are dried over sodium sulfate. Excess solvent and other volatilereaction components are completely removed under reduced pressure initially ona rotary evaporator and then under high vacuum(approximately 0.2 mm for 3 hr at 30°C). The resulting semi-solid is suspendedin 40 mL of ether andthe suspension is allowed to stand at room temperature overnight. The mixtureis stirred while 20 mL of hexanes is slowly added.The resulting white solid is filtered under vacuum and the filter cake iswashed with 200 mL of 50% (v/v) ether-hexanes.The solvent is removed from the filtrate on a rotary evaporator under reducedpressure to give a yellow oil that is dissolved in 10 mLof methylene chloride and diluted with 40 mL of 8% ether-hexanes. The solution isapplied to a flash chromatography column and eluted with 8%ether-hexanes to give 5.03 g (85.6%) of pure nitrobenzoate ester as a white crystallinesolid.

【Organic Syntheses,Coll. Vol. 9, p.607; Vol. 73, p.110.】

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