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With hydrogenchloride; In hexane; water; ethyl acetate; acetone;
EXAMPLE 1 To a well-stirred solution of 6.0 g (purity by 60 MHz NMR spectrum in acetone-d6 using 2,6-dichloroacetophenone as the reference: 97.35percent; 14.9 mmol) of 6,6-dibromo-penicillanic acid-1,1-dioxide in 150 ml of ethyl acetate and 35 ml of water kept at -2° to 3° C. was added portionwise 3.8 g of magnesium powder, while maintaining the pH of the reaction at 3.5 with 4N hydrochloric acid. The contents were stirred for another 2 hours while maintaining the pH at 3.5 with 4N hydrochloric acid and the temperature at -2° to 3° C. Then, the solid was filtered, washed with water and ethyl acetate and the combined filtrate was adjusted to a pH of 2.0 with 4N hydrochloric acid whereupon the layers were separated. The aqueous layer was extracted 3 times with 80 ml of ethyl acetate, after which the combined extracts were washed with brine (2* 60 ml), dried over anhydrous magnesium sulfate and filtered. The filtrate was evaporated to dryness under reduced pressure to obtain a white solid product which was taken up in n-hexane. The solution was filtered and the filtrate was evaporated to dryness under reduced pressure to obtain 3.125 g of penicillanic acid-1,1-dioxide with a purity by 360 MHz spectrum of 96.3percent giving a yield of 87percent.
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