反应详情

Into dimethyl sulfoxide (30 ml) were added (R)-2-(3-chlorophenyl)-2-hydroxyethyl methanesulfonate obtained in 2) above (10 g) and, under ice-cooling, a 5N aqueous NaOH solution (15 ml), and then the resulting mixture was stirred at the same temperature for 12 hours. The reaction mixture was added into ice water and extracted with 50% diethyl ether/pentane. The organic layer was washed with a saturated aqueous sodium chloride solution and then dried with anhydrous magnesium sulfate. The desiccant was filtered off, then the solvent was distilled off under reduced pressure, and the oily substance obtained was distilled under reduced pressure to obtain a colorless oily compound mentioned above (3.62 g, 76.5%). The optical purity of the product obtained was 97.5% e.e. as determined by HPLC.

1. customobtained in 2) above (10 g)
2. temperatureunder ice-cooling
3. extractionextracted with 50% diethyl ether/pentane
4. washThe organic layer was washed with a saturated aqueous sodium chloride solution
5. dry with materialdried with anhydrous magnesium sulfate
6. filtrationThe desiccant was filtered off
7. distillationthe solvent was distilled off under reduced pressure
8. customthe oily substance obtained
9. distillationwas distilled under reduced pressure
10. customto obtain a colorless oily compound
11. customThe optical purity of the product obtained