化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2013年
11期
2650-2654,2690
,共6页
张学勤%何年志%肖美添%叶静
張學勤%何年誌%肖美添%葉靜
장학근%하년지%초미첨%협정
2-氧-4-苯基丁酸乙酯%辛可尼定%铂%不对称加氢%聚乙烯吡咯烷酮%(R)-2-羟基-4-苯基丁酸乙酯
2-氧-4-苯基丁痠乙酯%辛可尼定%鉑%不對稱加氫%聚乙烯吡咯烷酮%(R)-2-羥基-4-苯基丁痠乙酯
2-양-4-분기정산을지%신가니정%박%불대칭가경%취을희필각완동%(R)-2-간기-4-분기정산을지
ethyl 2-oxo-4-phenylbutyrate%cinchonidine%platinum%asymmetric hydrogenation%polyvinylpyrrolidone%ethyl (R)-2-hydroxy-4-phenylbutyrate
分别采用乙醇、甲醛、甲酸钠、硼氢化钠为还原剂,聚乙烯吡咯烷酮(PVP)为稳定剂,制备了负载型PVP-Pt/γ-Al2O3催化剂,考察了催化剂对2-氧-4-苯基丁酸乙酯不对称加氢合成(R)-2-羟基-4-苯基丁酸乙酯的性能,其中硼氢化钠作为还原剂时性能最佳。研究了制备条件如还原温度、还原浓度、还原介质、PVP/Pt 物质的量比以及反应溶剂、时间等因素对催化结果的影响。实验结果表明,在 PVP/Pt=5∶1、还原温度0℃、NaBH4浓度为0.5 mol/L、乙醇作为还原介质制备的催化剂,对2-氧-4-苯基丁酸乙酯(EOPB)不对称加氢的转化率可达100%,对映选择性为76.8%e.e.。
分彆採用乙醇、甲醛、甲痠鈉、硼氫化鈉為還原劑,聚乙烯吡咯烷酮(PVP)為穩定劑,製備瞭負載型PVP-Pt/γ-Al2O3催化劑,攷察瞭催化劑對2-氧-4-苯基丁痠乙酯不對稱加氫閤成(R)-2-羥基-4-苯基丁痠乙酯的性能,其中硼氫化鈉作為還原劑時性能最佳。研究瞭製備條件如還原溫度、還原濃度、還原介質、PVP/Pt 物質的量比以及反應溶劑、時間等因素對催化結果的影響。實驗結果錶明,在 PVP/Pt=5∶1、還原溫度0℃、NaBH4濃度為0.5 mol/L、乙醇作為還原介質製備的催化劑,對2-氧-4-苯基丁痠乙酯(EOPB)不對稱加氫的轉化率可達100%,對映選擇性為76.8%e.e.。
분별채용을순、갑철、갑산납、붕경화납위환원제,취을희필각완동(PVP)위은정제,제비료부재형PVP-Pt/γ-Al2O3최화제,고찰료최화제대2-양-4-분기정산을지불대칭가경합성(R)-2-간기-4-분기정산을지적성능,기중붕경화납작위환원제시성능최가。연구료제비조건여환원온도、환원농도、환원개질、PVP/Pt 물질적량비이급반응용제、시간등인소대최화결과적영향。실험결과표명,재 PVP/Pt=5∶1、환원온도0℃、NaBH4농도위0.5 mol/L、을순작위환원개질제비적최화제,대2-양-4-분기정산을지(EOPB)불대칭가경적전화솔가체100%,대영선택성위76.8%e.e.。
A series of catalysts PVP-Pt/γ-Al2O3 were prepared by different reduction methods (ethanol, HCHO,HCOONa,and NaBH4) in the presence of PVP (polyvinylpyrrolidone) as stabilizer,the catalytic performance for asymmetric hydrogenation of ethyl 2-oxo-4-phenylbutyrate to ethyl (R)-2-hydroxy-4-phenylbutyrate was tested.The catalyst prepared by using NaBH4 as reducing agent showed the best overall performance.The effect of various catalyst preparation conditions,such as reduction temperature,NaBH4 concentration,the medium in which reduction was carried out, PVP/Pt mole ratio and reaction solvent and time,was also investigated. Ethyl (R)-2-hydroxy-4-phenylbutyrate could be obtained with 100%yield and 76.8%e.e. when catalyst was prepared at 0 ℃ using 0.5 mol/L NaBH4 in a medium of ethanol.