（＋）-（4S,5R）-and （-）-（4R,5S）-osmundalactones as well as （＋）-（4R,5S）- and （-）-（4S,5R）- 5-hydroxy-2-hexen-4-olides were synthesized by a concise and efficient synthesis method starting from 4-benzyloxy-...（＋）-（4S,5R）-and （-）-（4R,5S）-osmundalactones as well as （＋）-（4R,5S）- and （-）-（4S,5R）- 5-hydroxy-2-hexen-4-olides were synthesized by a concise and efficient synthesis method starting from 4-benzyloxy-5-hydroxy-2（E）-hexenoate in good yield with over 99% e.e..展开更多
本研究以3-丁炔-1-醇和苄溴为原料,合成3-炔-丁基苯甲醚,通过Sonogashira反应与5-碘胞苷合成得到(4-苄氧基)丁炔基-5-胞苷,其结构经核磁共振(1 H NMR和13 C NMR)以及质谱(MS)确证。最后通过研究极性、pH值以及粘度对其光谱性质的影响,...本研究以3-丁炔-1-醇和苄溴为原料,合成3-炔-丁基苯甲醚,通过Sonogashira反应与5-碘胞苷合成得到(4-苄氧基)丁炔基-5-胞苷,其结构经核磁共振(1 H NMR和13 C NMR)以及质谱(MS)确证。最后通过研究极性、pH值以及粘度对其光谱性质的影响,考察其是否具有成为极性、pH值以及粘度荧光探针的潜在价值。结果表明,在不同溶剂中(4-苄氧基)丁炔基-5-胞苷均有很强发射性。随着极性增加,荧光强度出现减小趋势;荧光强度随着粘度的变化而呈上升趋势;并且插入寡聚核酸中能够保持荧光性,不对周围环境产生影响。说明其该化合物在一定程度上有成为荧光探针的价值。展开更多
R)-Hydroxy-(S)-proline was N-protected by reaction with di-tert-butyl pyrocarbonate to give N-Boc-(4R)-hydroxy-(S)-proline, which was treated with NaH in anhydrous tetrahydrofuran and followed by etherification with P...R)-Hydroxy-(S)-proline was N-protected by reaction with di-tert-butyl pyrocarbonate to give N-Boc-(4R)-hydroxy-(S)-proline, which was treated with NaH in anhydrous tetrahydrofuran and followed by etherification with PhCH 2Br to form the N-Boc-(4R)-benzyloxy-(S)-proline, which, after removal of the protecting group with CF 3COOH gave the title compound. As an efficient catalyst for the direct asymmetryic aldol reaction the compound gave products in yield ranged from 58% to 77% with enantiomeric excess up to 88%.展开更多
The title compound 2（C22H28N＋O3）·H2O·2Cl-was synthesized by the reaction of 2-bromo-1-[4-（benzyloxy）phenyl]-1-pentone with 2,2＇-azanediyldiethanol. The crystal determined by X-ray diffraction analysis ...The title compound 2（C22H28N＋O3）·H2O·2Cl-was synthesized by the reaction of 2-bromo-1-[4-（benzyloxy）phenyl]-1-pentone with 2,2＇-azanediyldiethanol. The crystal determined by X-ray diffraction analysis belongs to the monoclinic system, space group Pc with a = 18.312（3）, b = 14.838（3）, c = 7.6227（14） , β = 97.981（4）°, Z = 2, Mr = 797.82, V = 2051.1（6） 3, Dc = 1.292 g/cm3, S = 0.956, μ = 0.21 mm-1, F（000） = 852, the final R = 0.0625 and wR = 0.1428 for 5683 observed reflections （Ⅰ 〉 2σ（Ⅰ））. Flack parameter is 0.10（9）. The title compound is composed by four non-coplanar ring systems, two benzenes and two morpholines. One morpholine ring （C（3）-C（4）-N（1）-C（1）-C（2）-O（1）） forms a chair conformation, while the other （C（4）-C（3）-O（2）-C（6）-C（5）-N（1）） assumes a boat conformation. X-ray crystal structure displays extensive N-H…Cl and O-H…Cl intermolecular hydrogen bonds. The preliminary antidepressant activity test indicates that the inhibition ratio of SERT （5-HT Transporter） was 35.9% at the dosage of 10.0 mg/L.展开更多
文摘（＋）-（4S,5R）-and （-）-（4R,5S）-osmundalactones as well as （＋）-（4R,5S）- and （-）-（4S,5R）- 5-hydroxy-2-hexen-4-olides were synthesized by a concise and efficient synthesis method starting from 4-benzyloxy-5-hydroxy-2（E）-hexenoate in good yield with over 99% e.e..
文摘本研究以3-丁炔-1-醇和苄溴为原料,合成3-炔-丁基苯甲醚,通过Sonogashira反应与5-碘胞苷合成得到(4-苄氧基)丁炔基-5-胞苷,其结构经核磁共振(1 H NMR和13 C NMR)以及质谱(MS)确证。最后通过研究极性、pH值以及粘度对其光谱性质的影响,考察其是否具有成为极性、pH值以及粘度荧光探针的潜在价值。结果表明,在不同溶剂中(4-苄氧基)丁炔基-5-胞苷均有很强发射性。随着极性增加,荧光强度出现减小趋势;荧光强度随着粘度的变化而呈上升趋势;并且插入寡聚核酸中能够保持荧光性,不对周围环境产生影响。说明其该化合物在一定程度上有成为荧光探针的价值。
文摘以间甲氧基苯酚为原料,通过氧烷基化及Vilsmeier-Hack(V-H)反应合成了4-苄氧基-2-甲氧基苯甲醛,总收率为82.26%.最佳反应条件为:以四丁基溴化铵为催化剂,合成间苄氧基苯甲醚的反应时间为3 h,n(间苄氧基苯甲醚)∶n(DMF)∶n(POCl3)=1∶1.5∶2,V-H反应温度为70—75℃,生成V-H试剂时间为1.5 h,保温反应时间为3 h.
文摘R)-Hydroxy-(S)-proline was N-protected by reaction with di-tert-butyl pyrocarbonate to give N-Boc-(4R)-hydroxy-(S)-proline, which was treated with NaH in anhydrous tetrahydrofuran and followed by etherification with PhCH 2Br to form the N-Boc-(4R)-benzyloxy-(S)-proline, which, after removal of the protecting group with CF 3COOH gave the title compound. As an efficient catalyst for the direct asymmetryic aldol reaction the compound gave products in yield ranged from 58% to 77% with enantiomeric excess up to 88%.
基金Project supported by the National Technology R&D Program (No. 2011 BAE06B01)
文摘The title compound 2（C22H28N＋O3）·H2O·2Cl-was synthesized by the reaction of 2-bromo-1-[4-（benzyloxy）phenyl]-1-pentone with 2,2＇-azanediyldiethanol. The crystal determined by X-ray diffraction analysis belongs to the monoclinic system, space group Pc with a = 18.312（3）, b = 14.838（3）, c = 7.6227（14） , β = 97.981（4）°, Z = 2, Mr = 797.82, V = 2051.1（6） 3, Dc = 1.292 g/cm3, S = 0.956, μ = 0.21 mm-1, F（000） = 852, the final R = 0.0625 and wR = 0.1428 for 5683 observed reflections （Ⅰ 〉 2σ（Ⅰ））. Flack parameter is 0.10（9）. The title compound is composed by four non-coplanar ring systems, two benzenes and two morpholines. One morpholine ring （C（3）-C（4）-N（1）-C（1）-C（2）-O（1）） forms a chair conformation, while the other （C（4）-C（3）-O（2）-C（6）-C（5）-N（1）） assumes a boat conformation. X-ray crystal structure displays extensive N-H…Cl and O-H…Cl intermolecular hydrogen bonds. The preliminary antidepressant activity test indicates that the inhibition ratio of SERT （5-HT Transporter） was 35.9% at the dosage of 10.0 mg/L.
