反应详情

One portion of sucrose octasulfate solution prepared as described in I above was adjusted with 10% w/w aqueous potassium hydroxide to pH=9 with stirring at room temperature. The solution was evaporated at 50° C. in vacuo to remove pyridine and water until 880 g were left. The warm solution was filtered, adjusted to pH=9.5, and the substance was precipitated with slow cooling to 5° C. The substance was filtered and washed with 300 ml of 1:1 ion-exchanged water/methanol and 300 ml of methanol. The wet filter cake was dried in vacuo at 50° C. The crude product was dissolved at 40° C. in 700 ml of ion-exchanged water. The liquid was filtered and adjusted to pH=9.5, and the substance was precipitated with slow cooling to 5° C. The precipitated substance was filtered and washed with 300 ml of 1:1 ion-exchanged water/methanol and 300 ml of methanol. The wet filter cake was dried in vacuo at 50° C. The substance was reprecipitated twice as mentioned above.

1. customThe solution was evaporated at 50° C. in vacuo
2. customto remove pyridine and water until 880 g
3. waitwere left
4. filtrationThe warm solution was filtered
5. customthe substance was precipitated
6. temperaturewith slow cooling to 5° C
7. filtrationThe substance was filtered
8. washwashed with 300 ml of 1:1 ion-exchanged water/methanol and 300 ml of methanol
9. customThe wet filter cake was dried in vacuo at 50° C
10. dissolutionThe crude product was dissolved at 40° C. in 700 ml of ion-exchanged water
11. filtrationThe liquid was filtered
12. customthe substance was precipitated
13. temperaturewith slow cooling to 5° C
14. filtrationThe precipitated substance was filtered
15. washwashed with 300 ml of 1:1 ion-exchanged water/methanol and 300 ml of methanol
16. customThe wet filter cake was dried in vacuo at 50° C
17. customThe substance was reprecipitated twice