Potassium Hydroxide → Octapotassium (2R,3R,4S,5R,6R)-2-(((2S,3S,4R,5R)-3,4-disulfato-2,5-bis(sulfatomethyl)oxolane-2-yl)oxy)-3,4,5-trisulfato-6-(sulfatomethyl)oxane

Participants

Reaction Steps

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.

Provenance & Evidence