反应详情

温度

7.5 °C

To a solution of phosphoric acid mono-(1-{4-[(S)-5-(acetylamino-methyl)-2-oxo-oxazolidin-3-yl]-2,6-difluorophenyl}-4-methoxymethyl-piperidin-4-yl)ester (5.0 g, 0.010mol) anhydrous methanol (50 ml) at 0-5° C., under argon, was added powdered anhydrous magnesium hydroxide (0.585 g, 0.010 mol) and water (5 ml) simultanously. The reaction mixture was stirred at 5-10° C. for 2 hours. The ice-bath was removed and the stirring continued further at 30-35° C. for 1 hour. The reaction mixture was filtered and the filtrate evaporated under reduced pressure. Acetone (25 ml) was added to the residue and triturated. The solvent was decanted. This procedure was repeated twice with acetone (50 ml). Acetone after the third trituration was decanted and the residue dried under reduced pressure to obtain the product as white solid, 4.9 g, in 92% yield, Mp>200° C. (dec); MF: C19H24F2MgN3O8P. Aqueous solubility at pH 7 was ˜2 mg/ml.

1. customThe ice-bath was removed
2. waitthe stirring continued further at 30-35° C. for 1 hour
3. filtrationThe reaction mixture was filtered
4. customthe filtrate evaporated under reduced pressure
5. additionAcetone (25 ml) was added to the residue
6. customtriturated
7. customThe solvent was decanted
8. customAcetone after the third trituration was decanted
9. customthe residue dried under reduced pressure