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氯法拉滨及其α异构体的合成 被引量:1
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作者 颜耀东 李强 +1 位作者 黄晓洁 邢雪忠 《解放军药学学报》 CAS 2012年第3期218-219,235,共3页
目的优化合成氯法拉滨及其α异构体的合成路线。方法以2-脱氧-2-β-氟-1,3,5-三-氧-苯甲酰基-α-D-呋喃核糖经溴化反应,再与2-氯腺嘌呤在叔丁醇钾作用下缩合后,碱性条件下脱去糖基保护基制得氯法拉滨(1)和氯法拉滨α异构体(6)。结果总... 目的优化合成氯法拉滨及其α异构体的合成路线。方法以2-脱氧-2-β-氟-1,3,5-三-氧-苯甲酰基-α-D-呋喃核糖经溴化反应,再与2-氯腺嘌呤在叔丁醇钾作用下缩合后,碱性条件下脱去糖基保护基制得氯法拉滨(1)和氯法拉滨α异构体(6)。结果总收率为28%,目标化合物的结构经IR、1HNMR、13CNMR、MS等方法确证。结论该合成工艺具有操作简便、产率较高、易于工业化生产等特点。 展开更多
关键词 氯法拉滨 氯法拉滨α异构体 合成
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Isolation and Characterization of R-Enantiomer in Ezetimibe 被引量:2
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作者 Kameswararao Chimalakonda Venugopal Kamani +2 位作者 Madhusudhan Gutta Srinivasulu Polisetty Sai Venkata Srinivas Koduri 《American Journal of Analytical Chemistry》 2013年第9期488-495,共8页
A simple and rapid Supercritical Fluid Chromatography (SFC) method has been developed to isolate and characterize R-Isomer of Ezetimi be by using normal phase Chiral Cel OD-H with 250 mm × 30 mm, 5 microns column... A simple and rapid Supercritical Fluid Chromatography (SFC) method has been developed to isolate and characterize R-Isomer of Ezetimi be by using normal phase Chiral Cel OD-H with 250 mm × 30 mm, 5 microns column using a mobile phase system containing super critical fluid carbondi oxide (Co2) and the percentage of 2-Propanol as a mobile phase (85:15) and detection at 230 nm. The isolated R-Isomer is characterized by using UV-vis, FT-IR, ESI-MS, HPLC1H and 13C NMR. The purity of isolated R-Isomer is about 98%. 展开更多
关键词 Isolation Characterization (R)-isomer EZETIMIBE SUPERCRITICAL Fluid Hromatography (SFC)
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Isolation and Characterization of S-Enantiomer in Montelukast 被引量:1
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作者 Vijaya Lakshmi Maddala Kishore Kumar Kakumani +2 位作者 Kameswara Rao Chimalakonda Srinivasulu Polisetty P. C. Ray 《American Journal of Analytical Chemistry》 2013年第1期56-61,共6页
A simple and rapid Supercritical Fluid Chromatography (SFC) Method has been developed to isolate and characterize the S-Isomer of Montelukast by using normal phase Amylose based AS-H with 250 mm × 30 mm, 5 micron... A simple and rapid Supercritical Fluid Chromatography (SFC) Method has been developed to isolate and characterize the S-Isomer of Montelukast by using normal phase Amylose based AS-H with 250 mm × 30 mm, 5 microns column using a mobile phase system containing super critical fluid carbon dioxide (CO2) and the percentage of 2-Propanol as a mobile phase (85:15) and detection at 230 nm. The isolated S-Isomer was characterized by using FT-IR, ESI-MS, HPLC and 1H NMR. The purity of isolated S-Isomer is about 98%. 展开更多
关键词 (S)-isomer MONTELUKAST SUPERCRITICAL Fluid Chromatography (SFC)
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Structure of Potassium of Undecatungstomononickelosilicate
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作者 Qu Lun-Yu Ma Rong-Hua +1 位作者 Chen Ya-Guang(Department of Chemistry, Northeast Normal University,Changchun 130024) Xing Yan Lin Yong-Hua(Changchun Institute of Applied Chemistry,Academia Sinica,Changchun 130022) 《Chinese Journal of Structural Chemistry》 SCIE CAS CSCD 1995年第6期51-54,共4页
The compound K<sub>4</sub>[α-SiNiW<sub>11</sub>O<sub>38</sub>]·10H<sub>2</sub>O,Mr=3053.86,crystallizes in the orthorhombic, space group Pnn2 with cell dimensions ... The compound K<sub>4</sub>[α-SiNiW<sub>11</sub>O<sub>38</sub>]·10H<sub>2</sub>O,Mr=3053.86,crystallizes in the orthorhombic, space group Pnn2 with cell dimensions a=14.203(8),b=14.214(6),c=12.460(3),V=2515(2),Z=2,Dc=4.03 g/cm ̄3,λ(MoKα)=0.71069,μ=273.1 cm(-1),F(000)=2672.The structure was solved by direct methods.The least-square refinement based on 1190 observed reflections[I】 6σ(I)] converged to a final R=0.076.The anion in the title compound is of α type Keggin structure,although the octahedron MO6 is greatly distorted. Atoms Ni and W are statistically distributed in the crystal. 展开更多
关键词 crystal structure α-isomer nickel-monosubstituted heteropoly compound
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