Hydrochloric Acid → HCID 15405224, compound

Participants

Reaction Steps

Into a four-mouthflask (volume: 100 ml) in which the inside was replaced by nitrogen were supplied diethyl ether (hereinafter referred to as "ether") and lithium aluminum hydride (0.2 g, 5.5 mmol). To this solution was added dropwise at room temperature an ether solution of 5,9-dimethyl-2-oxabicyclo-[4,4,0]-decan-3-one (0.1 g, 0.55 mmol) which had been separately prepared. The mixture was allowed to react at the same temperature for 1 hour, and the reaction solution was poured into a 10% aqueous hydrochloric acid solution for separation. The ether layer was separated, washed with brine, dried over anhydrous magnesium sulfate and concentrated. The resultant crude product was purified by column chromatography on silica gel to give the title compound (2) (80 mg) (Theoretical yield: 78.1%). Analytical results on the title compound are given below.

Provenance & Evidence