反应详情

温度

0 °C

A solution of 1.20 g, (1.73 mmol) phosphoric acid dibenzyl ester (3S,4S)-4-[2-(4-benzyl-3-hydroxy-piperidin-1-yl)-ethanesulfonyl]-phenyl ester in 40 ml MeOH and 6 ml water was hydrogenated at room temperature (20 bar, 5 h). The reaction mixture was concentrated to 20 ml and 500 ml water were added. The reaction mixture was filtered and the catalyst was washed with water. The filtrate was concentrated under reduced pressure until the product precipitates. The mixture was then cooled to 0° C. and 200 ml MeOH were added dropwise. After two hours the solid was filtered, washed with cold MeOH and dried at 60° C. under high vacuum to give 380 mg (0.83 mmol, 48%) of phosphoric acid mono-{(3S,4S)-4-[2-(4-benzyl-3-hydroxy-piperidin-1-yl)-ethanesulfonyl]-phenyl} ester as colorless crystalls.

1. customwas hydrogenated at room temperature
2. custom(20 bar, 5 h)
3. concentrationThe reaction mixture was concentrated to 20 ml and 500 ml water
4. additionwere added
5. filtrationThe reaction mixture was filtered
6. washthe catalyst was washed with water
7. concentrationThe filtrate was concentrated under reduced pressure until the product
8. customprecipitates
9. addition200 ml MeOH were added dropwise
10. filtrationAfter two hours the solid was filtered
11. washwashed with cold MeOH
12. customdried at 60° C. under high vacuum