Chemoselective hydrogenolysis of tetrahydrofurfuryl alcohol to 1,5-pentanediol over Ir-MoO_x/SiO_2 catalyst

In this work, MoOx promoted Ir/SiO2 catalysts were prepared and used for the selective hydrogenolysis of tetrahydrofurfuryl alcohol （THFA） to 1,5-pentanediol in a continuous flow reactor. The effects of different noble metals （Ir, Pt, Pd, Ru, Rh）, supports and Ir contents were screened. Among the investigated catalysts, 4 wt%Ir-MoOx/SiO2 with a Mo/Ir atomic ratio of 0.13 exhibited the best catalytic performance. The synergy between Ix particles and the partially reduced isolated MoOx species attached on them is essential for the excellent catalytic performance of Ix-MoOx/SiO2. The catalyst exhibited a better hydrogenolysis efficiency of THFA with the selectivity of 1,5-pentanediol of 65%-74% at a conversion of THFA of 70%-75% when the initial THFA concentration is ranging from 20 wt% and 40 wt%. And higher system pressure was also in favor of the conversion of THFA. During a stability test, the conversion of THFA and 1,5-pentanediol yield over Ix-MoOz/SiO2 decreased with reaction time, which can be explained by the leaching of Mo species during the reaction.

Environment-friendly synthesis of N-phenylpiperidine from aniline and 1,5-pentanediol overγ-Al_2O_3 catalyst

An efficient environment-friendly synthesis of N-phenylpiperidine was developed from aniline and 1,5-pentanediol over γ-Al2O3 catalyst under atmospheric pressure. The conversion of 1,5-pentanediol reached 97% and the selectivity for N-phenylpiperidine attained 94%. The structure of the catalyst was characterized by NH3-TPD and BET. The influences of calcination temperature of the catalyst and reaction temperature on activity and selectivity of the catalyst were investigated.

苯磺顺阿曲库铵注射液中1,5-戊二醇二丙烯酸酯含量的测定

目的建立苯磺顺阿曲库铵注射液中基因毒性杂质1,5-戊二醇二丙烯酸酯含量的HPLC方法。方法采用YMC-Ultra HT Hydrosphere C 18色谱柱(100 mm×3.0 mm,2μm),以0.2%磷酸水溶液为流动相A,乙腈为流动相B,进行梯度洗脱,流速为每分钟0.6 mL,柱温为30℃,检测波长为210 nm,研究苯磺顺阿曲库铵注射液中1,5-戊二醇二丙烯酸酯的含量测定。结果苯磺顺阿曲库铵注射液中1,5-戊二醇二丙烯酸酯与相邻色谱峰能达到有效分离;1,5-戊二醇二丙烯酸酯浓度在0.02~0.40μg·mL^(-1)内线性良好,分析方法的回收率、重复性与中间精密度、溶液的稳定性、耐用性等均在标准的规定范围内。结论该定量方法准确、可靠、稳定,可用于苯磺顺阿曲库铵注射液中1,5-戊二醇二丙烯酸酯的含量测定。