HCID 67927934, compound → HCID 67927932, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of Compound (3) (128.6 g; 458 mmol) in methanol (1400 ml), 1N aqueous sodium hydroxide (504 ml) was dropwise added while cooling at 0° C., and the resultant mixture was stirred at the same temperature for 1 hour and at room temperature for 3 hours, followed by concentration. The residue was diluted with a slight amount of water and washed with ether three times. The aqueous layer was collected, adjusted to pH 3 with 5% aqueous citric acid while cooling and extracted with ethyl acetate three times. The organic layer was washed with a saturated aqueous solution of sodium chloride three times, dried over anhydrous sodium sulfate and concentrated to give crude crystals. Recrystallization of said crude crystals from a mixture of ethyl acetate and petroleum ether gave Compound (4) (115.3 g; yield, 94%).

Provenance & Evidence