Sodium Bicarbonate → HCID 22237254, compound

Participants

Reaction Steps

A 3-L flask equipped with a stirrer was charged with 450 g (1.7 mols) of 2,5-bis(acetoxymethyl)-1,4-dithian and 1500 mL of methanol, to which 314.6 g (3.7 mols) of sodium hydrogen carbonate was added with stirring. The mixture was heated to a temperature at which methanol served as the reflux, at which it was held for 5 hours. It was then cooled to room temperature and filtered to remove the residue. Then, the resultant filtrate was transferred to a 3-L flask equipped with a stirrer, to which 20 g of activated carbon was added. The mixture was again heated to a temperature at which methanol served as the reflux, at which it was held for 30 minutes, and then cooled to room temperature and filtered. The resultant filtrate was concentrated by an evaporator, to obtain a colorless, oily product. It was purified by silica gel chromatography with ethyl acetate/n-hexane as the development medium, to obtain 298 g (yield: 97%) of the 2,5-bis(hydroxymethyl)-1,4-dithian, represented by the formula (1-2). It had 99.9% of purity, as determined by gas chromatography.

Provenance & Evidence