Sodium Hydroxide → HCID 24885944, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of sodium hydroxide (3 g, 0.075 mol) in water (25 ml) and methanol (25 ml), 3,9-dimethyl-3,9-bis(propionyloxymethyl)-2,4,8,10-tetraoxaspiro[5,5]undecane (6.5 g, 18 mmol) was slowly added, followed by stirring for 40 minutes at 60° C. After the solvent was distilled off under reduced pressure, the resultant concentrate residue was dissolved in acetonitrile/brine. The separated-off organic layer was concentrated under reduced pressure, and then ethyl acetate was added thereto. After the insoluble material was filtered out, the resultant filtrate was concentrated again under reduced pressure. The resultant concentrate residue was recrystallized from ethyl acetate/hexane, to give 3,9-dimethyl-3,9-bis(hydroxymethyl)-2,4,8,10-tetraoxaspiro[5,5]undecane (3.4 g, 13.7 mmol, yield 76%).

Provenance & Evidence