Sodium Carbonate → HCID 22325082, compound

Participants

Reaction Steps

A solution containing 11.4 g of triethyloxonium tetrafluoroborate and 40 ml of dichloromethane is added dropwise, at 0° C., to a suspension containing 1.54 g of the product obtained in Step 2, 10 g of disodium hydrogen phosphate and 120 ml of dichloromethane. After 20 hours at 20° C., 40 ml of 10% aqueous sodium carbonate solution are added. The mixture is separated and the aqueous phase is extracted with dichloromethane. The combined organic phases are dried over sodium sulphate and then concentrated to dryness. The residue is taken up in 1N aqueous hydrochloric acid and the resulting solution is left at 20° C. for 3 hours. The mixture is made alkaline with sodium carbonate and extracted with dichloromethane. The combined dichloromethane phases are dried over sodium sulphate and concentrated to dryness. Chromatography over silica gel (dichloromethane/tetrahydrofuran: 95/5) allows the desired product to be isolated.

Provenance & Evidence