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β-地西他滨合成工艺改进
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作者 季春伟 姚彤 +3 位作者 毛联岗 李林哲 李润莱 李树安 《精细化工》 EI CAS CSCD 北大核心 2021年第9期1867-1874,1887,共9页
以2-脱氧-D-核糖为起始原料,用乙醇/乙酰氯替代甲醇/HCl,进行缩醛反应得到1-乙氧基-2-脱氧核糖;以二氯甲烷作为溶剂,用对氯苯甲酰氯代替对甲基苯甲酰氯保护1-乙氧基-2-脱氧核糖的3,5-二羟基得到1-乙氧基-2-脱氧-3,5-二对氯苯甲酰氧基-D... 以2-脱氧-D-核糖为起始原料,用乙醇/乙酰氯替代甲醇/HCl,进行缩醛反应得到1-乙氧基-2-脱氧核糖;以二氯甲烷作为溶剂,用对氯苯甲酰氯代替对甲基苯甲酰氯保护1-乙氧基-2-脱氧核糖的3,5-二羟基得到1-乙氧基-2-脱氧-3,5-二对氯苯甲酰氧基-D-呋喃核糖,1-乙氧基-2-脱氧核糖转化率为100.00%,并用低温析晶方法除去过量对氯苯甲酰氯;再经5′-氮杂胞嘧啶与糖苷缩合反应,氨甲醇脱保护反应,分离异构体得到β-地西他滨。采用^(1)HNMR、^(13)CNMR、MS、FTIR和X单晶衍射仪对产物及中间体的结构进行了表征。小试总收率达到30.62%,经千克级放大实验,β-地西他滨的总收率为30%以上。 展开更多
关键词 β-地西他滨 乙缩醛化 对氯苯甲酰氯 改进工艺 医药原料
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Catalytic upgrading of ethanol to butanol over a binary catalytic system of FeNiO_x and LiOH 被引量:1
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作者 Jifeng Pang Mingyuan Zheng +5 位作者 Zhinuo Wang Shimin Liu Xinsheng Li Xianquan Li Junhu Wang Tao Zhang 《Chinese Journal of Catalysis》 SCIE EI CAS CSCD 北大核心 2020年第4期672-678,共7页
Catalytic conversion of ethanol to butanol is vital to bridge the gap between huge amounts of ethanol production,the limited blending ratio of ethanol in gasoline,and the outstanding performance of butanol.In this wor... Catalytic conversion of ethanol to butanol is vital to bridge the gap between huge amounts of ethanol production,the limited blending ratio of ethanol in gasoline,and the outstanding performance of butanol.In this work,a highly active binary catalytic system of FeNiOx and LiOH was developed for upgrading of ethanol to butanol.After 24 h reaction at 493 K,the selectivity to butanol reached 71% with>90% high carbon alcohols at 28% ethanol conversion,which was comparable to the performance of some noble metal homogeneous catalysts. 展开更多
关键词 ETHANOL CATALYSIS BUTANOL Hydrogen transfer CONDENSATION
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The biomimetic catalytic synthesis of acetal compounds using β-cyclodextrin as catalyst 被引量:1
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作者 Daohong Xia Shengjuan Jiang +2 位作者 Lantao Li Yuzhi Xiang Lijun Zhu 《Chinese Journal of Chemical Engineering》 SCIE EI CAS CSCD 2016年第1期146-150,共5页
Based on the principle of biomimetic catalysis, β-cyclodextrin was applied to the acetalation reaction as a facile and efficient catalyst, and the synthesis was environmentally friendly with atomic economy. The influ... Based on the principle of biomimetic catalysis, β-cyclodextrin was applied to the acetalation reaction as a facile and efficient catalyst, and the synthesis was environmentally friendly with atomic economy. The influencing factors of the acetalation reaction e.g. the reaction time, the volume of water-carrying agent,the molar ratio of catalyst to benzaldehyde and the molar ratio of glycol to benzaldehyde had been studied.The yield of benzaldehyde glycol acetal would reach a maximum of 81.3% under the conditions approached.Six of other acetals were also synthesized. Moreover, a plausible reaction mechanism for the formation of acetal had been proposed. 展开更多
关键词 β-Cyclodextrin Biomimetic catalysis Synthesis Acetal
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Catalytic synthesis of benzaldehyde glycol acetal over H3PW6Mo6O40/PAn
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作者 YANG Shui-jin GAO Fei LV Bao-lan 《Journal of Chemistry and Chemical Engineering》 2008年第6期29-32,共4页
Catalytic activities of H3PWrMo6O40/PAn in synthesizing benzaldehyde glycol acetal were reported. It has been demonstrated that H3PW6MorO40/PAn is an excellent catalyst. Various factors concerned in the reaction have ... Catalytic activities of H3PWrMo6O40/PAn in synthesizing benzaldehyde glycol acetal were reported. It has been demonstrated that H3PW6MorO40/PAn is an excellent catalyst. Various factors concerned in the reaction have been investigated. The optimum conditions have been found, that is, the molar ratio of benzaldehyde to glycol is 1/1.4, the mass ratio of the catalyst used to the reactants is 0.8%, and the reaction time is 45min. Under these conditions, the yield of benzaldehyde glycol acetal is 79.0%. 展开更多
关键词 benzaldehyde glycol acetal H3PWrMo6O40/PAn POLYANILINE aetalization
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Synthesis, Characterization and Catalytic Application of H3PW12O40/MCM-48 in the Acetalization of Butyraldehyde with Glycol
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作者 Shuijin Yang Weiping Wang Baolan Lv 《Journal of Chemistry and Chemical Engineering》 2010年第4期29-33,共5页
A novel environmental friendly catalyst, H3PW12O40/MCM-48, was prepared by impregnation method. The catalysts were characterized by means of XRD and FT-IR. The synthesis of butyraldehyde glycol acetal catalyzed by H3P... A novel environmental friendly catalyst, H3PW12O40/MCM-48, was prepared by impregnation method. The catalysts were characterized by means of XRD and FT-IR. The synthesis of butyraldehyde glycol acetal catalyzed by H3PW12O40/MCM-48 was studied with butyraldehyde and glycol as reactants. H3PW12O40/MCM-48 was an excellent catalyst for the synthesizing butyraldehyde glycol acetal and Keggin structure of H3PW12O40 kept unchanged after being impregnated on surface of the molecular sieve support. Effects of n(butyraldehyde): n(glycol), catalyst dosage, cyclohexane(water-stripped reagent) and reaction time on yields of the product were investigated. The optimum conditions had been found, that was, molar ratio of butyraldehyde to glycol was 1: 1.6, mass ratio of catalyst used to the reactants was 0.25% and reaction time was 75 min. Under these conditions, the yield of butyraldehyde glycol acetal can reach 79.74%. 展开更多
关键词 MCM-48 molecular sieve phosphotungstic acid butyraldehyde glycol acetal CATALYSIS acetalization.
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