Preparation method for high purity racemic adrenaline
Abstract:
Disclosed is a preparation method for a racemic adrenaline as represented by formula II. The method comprises the following steps: compound 1 is directly racemized in an acidic solution to produce compound 2, the acid solution comprising neither sodium bisulfite nor salicylic acid; and specifically comprises (a), in the acid solution of which the pH is 0.5-1.5, compound 1 is placed under the protection of nitrogen gas and, with the reaction temperature being controlled at 75-95° C., stirred and reacted for 1-3 hours; (b) the reaction solution is controlled at a temperature of 5-20° C., into which an activated carbon is added, under the protection of nitrogen gas, stirred for 20-40 minutes, and filtered, then a filtrate is collected; the filtrate is controlled at a temperature of 5-20° C., the pH thereof is adjusted using ammonia to 8.5-9.5, and is filtered when the pH is stabilized, and a filter cake is washed and dried to produce a high purity racemic adrenaline white powder. The weight yield of the product produced per the preparation method of the present invention is greater than 90%, the chromatographic purity is greater than 96%, and the ee value approaches zero; the invention is inexpensive, simple to operate, favors industrialized production, and has a broad application prospect.
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