4-Methylenepiperidine hydrochloride 1 is a key intermediate for synthesis of the novel antifungal drug efinaconazole 2. In this work, a simple and robust process has been developed to synthesize 4-methylenepiperidine hydrochloride 1, with a high overall yield of 99.1% at a high purity of 99.7% in a large-scale. Moreover, this synthetic process avoided the uses of organolithium reagent and column chromatography process which are not desirable for industrial production.

Shandong Huagong

Determination of genotoxic impurities in ganciclovir condensates by HPLC

Author: Wang, Jian ; Xu, Yutian ; Fan, Huayu ; Wu, Ke ; Cao, Li

Objective: To establish a HPLC method for the determination of two potential genotoxic impurities Me toluenesulfonate and Et toluenesulfonate in ganciclovir condensates.Methods: Agilent Eclipse Plus C₁₈ column (250 mm × 4.6 mm, 5 μm) was used with 0.1% phosphoric acid aqueous solution as mobile phase A and acetonitrile as mobile phase B.Diode array detector was used to detect the two targets at the detection wavelength of 225 nm.Results: There was a linear relationship between the peak areas of the two kinds of target substances in a certain range of mass concentration, and the detection limits (3 S/N) were 15.852 and 15.848 ng·mL^-1, resp.The recoveries of actual samples were 101.3% ∼ 106.0% and 103.1% ∼ 106.7%, resp.Conclusion: This method is suitable for the determination of Me p-methylbenzenesulfonic acid and Et p-methylbenzenesulfonic acid in ganciclovir condensates.

Jingxi Yu Zhuanyong Huaxuepin

Synthesis of rabeprazole

Author: Wang, Zhi-hui ; Ao, Chen

A one-pot synthesis of 2-{[3-methyl-4-(3-methoxy-propoxyl)-2-pyridinyl] methyl-sulfinyl}-1H-benzimidazole from 2-(hydroxymethyl)-4-(3-methoxypropoxy)-3-methylpyridium hydrochloride was carried out via the chlorination reaction and condensation reaction, and then by oxidation, the target product rabeprazole was produced.

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