Sodium Bicarbonate → HCID 9808300, compound

Participants

Reaction Steps

The product of example 1 or example 7 (15.0 g, 26.0 mmol), dichloromethane (150 mL) and 5% w/v aqueous sodium hydrogen carbonate solution (150 mL) were combined and the resultant mixture was well stirred for 25 min at 35° C. Dichloromethane (100 mL) was then added and stirring was continued for 20 min. at 30° C. The reaction mixture was extracted with dichloromethane (2×100 mL), separated from the aqueous layer and the combined organic layer washed with water (4×200 mL). The washed organic layer was dried over anhydrous sodium sulfate, filtered and concentrated under vacuum to approximately 100 mL. To the concentrate thus obtained acetonitrile (500 mL) was added, crystallization was initiated during this addition, and the resultant crystal slurry further concentrated under vacuum to remove the remainder of the dichloromethane. This solid was filtrated and dried in a vacuum oven at 60° C.

Provenance & Evidence