反应详情

To the solution of sodium salt of di-protected Ertapenem (IV) (50 g) in carbonic acid water (500 ml), THF (100 ml), DMF (25 ml) and ethyl acetate (1000 mL) and sodium bicarbonate (6.5 gm) in autoclave, Pd/carbon charged and subjected to hydrogenation with 8 to 10 Kg pressure at 5-10° C. After completion of reaction CO2 gas was purged, the reaction mass was filtered. The aqueous layer was separated, washed with ethyl acetate and the residual solvents in aqueous layer removed using degassing technique. The pH of the aqueous layer was adjusted using acetic acid to about 5.5-7.0 and slowly added into mixture of methanol (400 ml) and absolute isopropyl alcohol (6 L) under stirring. The precipitated Ertapenem disodium was filtered, washed with IPA and dried to yield amorphous form of Ertapenem disodium of formula (I). The solid obtained was optionally treated with methanol/isopropyl ether mixture at about −20° C. to yield Ertapenem disodium with low residual solvent content.

1. customsubjected to hydrogenation with 8 to 10 Kg pressure at 5-10° C
2. customwas purged
3. filtrationthe reaction mass was filtered
4. customThe aqueous layer was separated
5. washwashed with ethyl acetate
6. customthe residual solvents in aqueous layer removed
7. customusing degassing technique
8. additionslowly added into mixture of methanol (400 ml) and absolute isopropyl alcohol (6 L)
9. filtrationThe precipitated Ertapenem disodium was filtered
10. washwashed with IPA
11. customdried