反应详情

1000 mg (1.84 mmol) of the compound from Example 39A are dissolved in 100 ml of dioxane, 150 mg (1.41 mmol) of palladium-on-activated carbon are added and the mixture is hydrogenated with hydrogen at 3 bar. After 3 h, 4 ml of 2M hydrochloric acid are added and the mixture is hydrogenated with hydrogen at 3 bar for a further 20 h. The mixture is then filtered off with suction through a Seitz clarifying sheet filter, the product is then washed with 50 ml of dioxane, and 50 ml of toluene are added to the filtrate. After removal of the solvent on a rotary evaporator, the residue is taken up in a mixture of 50 ml of water and 50 ml of ethyl acetate. By cautious addition of aqueous dilute sodium bicarbonate solution, the pH is adjusted to about pH 9. The phases formed are separated. The organic phase is dried over magnesium sulphate, the solvent is then removed using a rotary evaporator and the residue is purified by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5, with addition of 0.5% concentrated hydrochloric acid). The product-containing fractions are combined and concentrated using a rotary evaporator.

1. filtrationThe mixture is then filtered off with suction through a Seitz clarifying sheet
2. filtrationfilter
3. washthe product is then washed with 50 ml of dioxane, and 50 ml of toluene
4. additionare added to the filtrate
5. customAfter removal of the solvent
6. customon a rotary evaporator
7. additionthe residue is taken up in a mixture of 50 ml of water and 50 ml of ethyl acetate
8. additionBy cautious addition of aqueous dilute sodium bicarbonate solution
9. customThe phases formed
10. customare separated
11. dry with materialThe organic phase is dried over magnesium sulphate
12. customthe solvent is then removed
13. customa rotary evaporator
14. customthe residue is purified by preparative HPLC (column: YMC GEL ODS-AQ S-5/15 μm; mobile phase gradient: acetonitrile/water 10:90→95:5, with addition of 0.5% concentrated hydrochloric acid)
15. concentrationconcentrated
16. customa rotary evaporator