反应详情

温度

2.5 °C

Esomeprazole-BINOL inclusion complex (100 g; 158.3 mmol; ee of 98.2%) was suspended in a mixture of methyl t-butyl ether (1300 ml) and DM water (400 ml). Aqueous sodium hydroxide solution (5 w/w; 133 g) was added to the suspended mass at 20-30° C. and stirred till clear solution was obtained. Thereafter, organic layer was separated and the aqueous layer was washed with methyl t-butyl ether. Thereafter, 20% aqueous ammonium formate solution (60 ml) was added and extracted with methylene chloride (300 ml). The organic layer was washed with DM water and concentrated under reduced pressure to yield a foamy mass. The concentrated mass was dissolved in ethylacetate (400 ml) and cooled to 0-5° C. To the solution, sodium ethoxide (10.77 g, mmol) was added and stirred at 20-30° C. for 90 min. The separated solid mass was filtered, washed with ethyl acetate and dried under reduced pressure at 40° C. to yield esomeprazole sodium.

1. customwas obtained
2. customThereafter, organic layer was separated
3. washthe aqueous layer was washed with methyl t-butyl ether
4. additionThereafter, 20% aqueous ammonium formate solution (60 ml) was added
5. extractionextracted with methylene chloride (300 ml)
6. washThe organic layer was washed with DM water
7. concentrationconcentrated under reduced pressure
8. customto yield a foamy mass
9. stirringstirred at 20-30° C. for 90 min
10. filtrationThe separated solid mass was filtered
11. washwashed with ethyl acetate
12. customdried under reduced pressure at 40° C.