反应详情

A solution of 7.0 g of 2-(1-(iminomethyl)piperidin-4-yl)ethyl(2R)-2-((1R)-3,3-difluorocyclopentyl)-2-hydroxy-2-phenylethanoate monohydrochloride in 50 ml of ultrapure water was developed on reversed phase medium pressure liquid chromatography [ODS-AQ 120-S50 (YMC Co.)], and 300 ml of 1.0 M aqueous sodium dihydrogenephosphate solution, 300 ml of 0.2 M phosphoric acid and 300 ml of ultrapure water were flowed by the order stated, followed by elution with tetrahydrofuran/water=1/9. Distilling the solvent off under reduced pressure, the residue was crystallized in ethanol and recovered by filtration, to provide 6.5 g of the title compound as a colorless solid.

1. washfollowed by elution with tetrahydrofuran/water=1/9
2. distillationDistilling the solvent off under reduced pressure
3. customthe residue was crystallized in ethanol
4. filtrationrecovered by filtration