Water → HCID 178488037, compound

Temperature

31 °C

50 ml of methanol was taken into a round bottom flask and a mixture of 12.75 g sodium hydroxide and 11 ml of water was added to it and stirred for clear dissolution at 31° C. 110 g of esomeprazole was dissolved in 550 ml of methanol and the solution was added to the above methanolic sodium hydroxide solution. The mass was subjected to stirring at a temperature of 30° C. for 40 minutes, followed by the addition of 5.5 g of carbon with simultaneous stirring. The reaction mass was filtered through a Celite bed, and washed with 550 ml of methanol. The filtrate was subjected to distillation at a temperature of 30° C. under a vacuum of 200 torr. The residue was co-distilled with 1650 ml of acetone in three equal lots at 35° C. To the obtained residue, 220 ml of acetone was added and stirred for one hour. The separated solid was filtered and dried at 34° C. for 12 hours to afford 61.5 g of the title compound.

1. additionwas added to it
2. stirringto stirring at a temperature of 30° C. for 40 minutes
3. additionfollowed by the addition of 5.5 g of carbon with simultaneous stirring
4. filtrationThe reaction mass was filtered through a Celite bed
5. washwashed with 550 ml of methanol
6. distillationThe filtrate was subjected to distillation at a temperature of 30° C. under a vacuum of 200 torr
7. customwas co-distilled with 1650 ml of acetone in three equal lots at 35° C
8. additionTo the obtained residue, 220 ml of acetone was added
9. stirringstirred for one hour
10. filtrationThe separated solid was filtered
11. customdried at 34° C. for 12 hours

ORD record

ord-1dfd07f4b97a4e87886169b93cbd3470

Source dataset

uspto-grants-2011_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08063074B2