反应详情

One portion of sucrose octasulfate solution prepared as described in I above was adjusted with 10% w/w aqueous sodium hydroxide to pH=9 with stirring at room temperature. The solution was evaporated at 50° C. in vacuo to remove pyridine and water. When 250 ml were distilled, 580 ml of ethylene glycol were added and the evaporation was continued until 10 mm vacuum. 100 ml of ethanol were added to the solution. The solution was filtered, and pH was adjusted to 9.5. 350 ml of ethanol were slowly added with vigorous stirring at 30°-35° C., and the substance will then precipitate. After the addition was ended, the mixture was cooled to 10° C., and the solid substance was filtered and washed with 50 ml of 1:1 ethanol/ethylene glycol and 200 ml of methanol. The wet filter cake was dried in vacuo at 50° C. The crude product was dissolved in 520 ml of ethylene glycol and heated to 40° C., and 100 ml of ethanol were added. The solution was filtered and pH was adjusted to 9.5. 350 ml of ethanol were slowly added with vigorous stirring at 30°-35° C. and the substance will then precipitate. After the addition was ended, the mixture was cooled to 10° C. and the solid substance was filtered. It was washed with 50 ml of 1:1 ethanol/ethylene glycol and 200 ml of ethanol. The wet filter cake was dried in vacuo at 50° C.. The substance was reprecipitated once as above and then dried for 2 hours at room temperature in 500 ml of ethanol. The substance was filtered, washed with 200 ml of ethanol and dried at 50° C. in vacuo.

1. customThe solution was evaporated at 50° C. in vacuo
2. customto remove pyridine and water
3. distillationWhen 250 ml were distilled
4. addition580 ml of ethylene glycol were added
5. customthe evaporation
6. addition100 ml of ethanol were added to the solution
7. filtrationThe solution was filtered
8. addition350 ml of ethanol were slowly added
9. stirringwith vigorous stirring at 30°-35° C.
10. customthe substance will then precipitate
11. additionAfter the addition
12. temperaturethe mixture was cooled to 10° C.
13. filtrationthe solid substance was filtered
14. washwashed with 50 ml of 1:1 ethanol/ethylene glycol and 200 ml of methanol
15. customThe wet filter cake was dried in vacuo at 50° C
16. dissolutionThe crude product was dissolved in 520 ml of ethylene glycol
17. temperatureheated to 40° C.
18. addition100 ml of ethanol were added
19. filtrationThe solution was filtered
20. addition350 ml of ethanol were slowly added
21. stirringwith vigorous stirring at 30°-35° C.
22. customthe substance will then precipitate
23. additionAfter the addition
24. temperaturethe mixture was cooled to 10° C.
25. filtrationthe solid substance was filtered
26. washIt was washed with 50 ml of 1:1 ethanol/ethylene glycol and 200 ml of ethanol
27. customThe wet filter cake was dried in vacuo at 50° C.
28. customThe substance was reprecipitated once as above and
29. dry with materialthen dried for 2 hours at room temperature in 500 ml of ethanol
30. filtrationThe substance was filtered
31. washwashed with 200 ml of ethanol
32. customdried at 50° C. in vacuo