Su Yang,Xiaoxuan Guo,Xiaomei Pan,Liuyu Gu,Xueping Liu,Lijing Gao,Guomin Xiao
Concentrated sulfuric acid is generally used as a catalyst for producing brominated alkanes in traditional methods, but is highly corrosive and difficult to separate. This work reports the preparation of bromopropane from n-propanol based on a reactive distillation strategy combined with alumina-modified sulfated zirconia (Al2O3/SO42−/ZrO2) as a heterogenous catalyst. As expected, under the optimum reaction conditions (110 °C), the yield of bromopropane was 96.18% without side reactions due to the reactive distillation strategy. Meanwhile, the microscopic morphology and performance of Al2O3/SO42−/ZrO2were evaluated by X-ray diffraction (XRD), scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), Brunner–Emmet–Teller (BET), Fourier transform infrared spectroscopy (FT–IR), and other characterization methods. The results confirmed that the morphology of zirconia sulfate is effectively regulated by the modification method of alumina, and more edges and angles provide more catalytic acid sites for the reaction. Furthermore, Al2O3/SO42−/ZrO2exhibited high stability and remarkable reusability due to the strong chemical bond Zr–Al–Zr. This work provides a practical method for the preparation of bromopropane and can be further extended to the preparation of other bromoalkanes.Keywords:sulfated zirconia;modification of alumina;bromopropane;catalytic distillation
A sensitive and selective gas chromatography–tandem mass spectrometry method was developed for the identification and quantification of five potential genotoxic impurities (PGIs), i.e., chloromethane, 2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate, in abiraterone acetate. The method was validated according to the International Council for Harmonisation (ICH) guidelines. The linearity was established for the concentration range of 30–480 ng/mL (2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate) and 90–1440 ng/mL (chloromethane). The correlation coefficient of each PGIs was >0.995. The extraction recoveries ranged from 90.49 to 106.79% for the five PGIs. The quantitation limit, detection limit, accuracy, precision, repeatability and stability of the method demonstrated that the method was an adequate quality control tool for quantitation and identification of chloromethane, 2-chloropropane, 2-bromopropane, 4-chloro-1-butanol and diethyl sulfate at trace levels in drug substances and drug products.
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