Hydrochloric Acid → HCID 14025168, compound

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Reaction Steps

Dimethylacetal (3.04 g) obtained in Example 1 was dissolved in 30 ml of acetone, 2 ml of 6N hydrochloric acid was dropped therein with ice cooling and stirring, and the mixture was kept at 5° C. in a refrigerator for 4 days. To the reaction solution was added 30 ml of ice water, the mixture was neutralized with sodium bicarbonate, concentrated in vacuo at room temperature, the residual solution was extracted with chloroform, the chloroform layer was washed with sodium chloride solution, evaporated to dryness, the residue was purified by subjecting to a flash column chromatography, and the 1.38 g of resulting crude crystals were recrystallized from etherethyl acetate to give yellow prisms. M.p. 135°-136° C.

Provenance & Evidence