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为定量控制降糖药达格列净中的杂质,对达格列净中的2个杂质5-溴-2-氯-2′-乙氧基二苯甲酮(1)和5-溴-2-氯-2′-乙氧基二苯甲烷(2)进行了定向合成,以5-溴-2-氯苯甲酸和苯酚经缩合、Fries重排,然后乙基化得到杂质1,杂质1再经还原得到杂质2。其结构经核磁共振氢谱和质谱确证结构。
To quantitatively control the impurities in the hypoglycemic drug dapagliflozin, two impurities, 5-bromo-2-chloro-2’-ethoxybenzophenone (1) and 5- 2-chloro-2’-ethoxydiphenylmethane (2) were synthesized by condensation of Fries rearranged with 5-bromo-2-chlorobenzoic acid and phenol and then ethylated to give impurity 1, impurity 1 Then by reducing the impurities 2. Its structure was confirmed by 1H-NMR and MS-MS.