反应详情

温度

27 °C

20 g of meropenem-PNB was dissolved in 200 mL of tetrahydrofuran. 60 g of potassium phosphate monobasic (KH2PO4) dissolved in 400 mL of water was added thereto and heated to 27° C. 80 g of zinc powder was slowly added portionwise and stirred between 25 to 35° C. for 1 hour. After the completion of the reaction was confirmed, 220 mL of methylene chloride was added and stirred for 10 minutes, and then filtered to remove zinc powder. The aqueous layer was separated and washed 2 times with 100 mL of methylene chloride, by which tetrahydrofuran present in the aqueous layer was removed completely. The aqueous layer was cooled and developed in a column filled with adsorption resin SP-207 for adsorption. The resin column was washed with 2 L of water to remove potassium phosphate salt used in the reaction and impurities, and developed with 2 L of 60% methanol to elute meropenem completely. The fractions containing meropenem were collected and a buffer solution of N-methylmorpholine/acetic acid (pH 6.5) was added thereto, and concentration was conducted to a volume 10 times greater than the weight of meropenem-PNB. 1100 mL of acetone was added to generate crystal and stirred at room temperature for 1 hour. After filtration and drying, 9.78 g of meropenem trihydrate was obtained.

1. additionwas added
2. stirringstirred for 10 minutes
3. filtrationfiltered
4. customto remove zinc powder
5. customThe aqueous layer was separated
6. washwashed 2 times with 100 mL of methylene chloride
7. customby which tetrahydrofuran present in the aqueous layer was removed completely
8. temperatureThe aqueous layer was cooled
9. additionfilled with adsorption resin
10. washThe resin column was washed with 2 L of water
11. customto remove potassium phosphate salt
12. customused in the reaction and impurities
13. washto elute meropenem completely
14. additionThe fractions containing meropenem
15. customwere collected
16. additiona buffer solution of N-methylmorpholine/acetic acid (pH 6.5) was added
17. concentrationconcentration
18. addition1100 mL of acetone was added
19. stirringstirred at room temperature for 1 hour
20. filtrationAfter filtration
21. customdrying