含1,2,3-三氮唑哌啶衍生物的合成

1,2,3-三氮唑环作为药效基团呈现出多种生物活性,以六氢吡啶和环氧氯丙烷为底物,在微波辐射条件下,合成了叠氮基哌啶,并以此为原料,CuI为催化剂,MeCN-H2O(10∶1,v/v)为混合溶剂,与端基炔烃进行1,3-偶极环加成反应,合成含1,2,3-三氮唑功能基的哌啶衍生物,收率70%,其结构经核磁共振谱表征。     

1,4-二取代-1,2,3-三氮唑的合成研究

以苄基氯(1a)、4-氯苄基氯(1b)、特戊酸氯甲酯(1c)为原料,通过叠氮取代和1,3-偶极环加成反应合成了三种含羟基的三氮唑衍生物1-苄基-4-羟甲基-1H-1,2,3-三氮唑(3a)、1-(4-氯-苄基)-4-羟甲基-1 H-1,2,3-三氮唑(3 b)、1-(特戊酸甲酯基)-4-羟甲基-1 H-1,2,3-三氮唑(3 c),实验应用FT-IR、1HNMR、13CNMR对产物的结构进行了表征,结果证实了合成路线的可行性,目标产物的收率分别为85.32%、90.26%、72.62%。     

1H-1,2,3-三氮唑的合成改进

本研究以苄基氯、叠氮化钠、乙炔气体为原料,以铜催化下环加成为关键反应制备得1-苄基-1,2,3-三唑中间体,该中间体在钯/碳催化氢化下合成1H-1,2,3-三氮唑,总产率为70%。该方法反应条件温和,三废排放少。     

利用分子内环丙烷化反应合成四氢喹啉衍生物

报道了一种高效的基于三氮唑的分子内环丙烷化合成四氢喹啉并环丙烷骨架的新方法。利用邻烯基苯胺取代的1-磺酰基-1,2,3-三氮唑为原料,以Rh2(piv)4为催化剂,1,2-二氯乙烷为溶剂,在氮气氛下50摄氏度反应,以中等至优秀的产率得到四氢喹啉并环丙烷骨架。该反应巧妙利用了含氮原子的连接桥,操作简单,反应条件温和。     

1H-1,2,3-三氮唑的合成

研究了1H-1,2,3-三氮唑的新的合成工艺,以水合肼,盐酸羟胺,乙二醛为原料,经肟化、腙化、脱乙酰基等反应进行制备、优化。该新路线与传统工艺相比,全部采用工业原料,价格低,生产成本低,易于工业化,1H-1,2,3-三氮唑含量99.6%(色谱法)。     

叠氮基吡啶及1-吡啶基-1,2,3-三氮唑的合成

叠氮基吡啶是一类重要的有机化合物,其用途十分广泛,可用来构建含氮杂环化合物,合成除草剂等,介绍了叠氮基吡啶和1-吡啶基-1,2,3-三氮唑的合成方法及用途。     

利用三氮唑的4+3环化反应合成1,4-氧氮杂?

报道了一种合成1,4-氧氮杂?的新方法。利用1-磺酰基-1,2,3-三氮唑与α,β-不饱和醛为原料,以Rh_2(Oct)_4为催化剂,1,2-DCE为溶剂,在氮气氛下回流,以中等产率得到非苯并氧氮杂?衍生物。该反应经α-亚胺基铑卡宾的4+3成环历程,设计新颖,操作简单。     

合成1-(4-苯基-1,2,3-三氮唑-1-亚甲基)苯并三氮唑的新方法

三氮唑类衍生物具有抗菌、抗炎、抑制病毒生长等广泛的生物活性。从苯并三氮唑出发,通过点击化学反应在水相中合成了1-(4-苯基-1,2,3-三氮唑-1-亚甲基)苯并三氮唑,产率为91%;该合成方法具有简便快速、产率高等优点。     

糖基化三氮唑修饰的水杨醛席夫碱衍生物的合成与表征

以乙酰葡萄糖叠氮、3-溴丙炔、水杨醛和9种芳胺为原料,依据拼合原理设计合成了将糖苷、1,2,3-三氮唑和席夫碱3个药效基团构建于同一分子中的9个糖基化三氮唑水杨醛席夫碱衍生物,产物结构经1HNMR、IR、EI-MS和元素分析确认。     

杀菌剂戊环唑的合成研究

以间二氯苯,乙二醇,ＩＨ-１,２,４-三氮唑等为原料,成戊环唑的合成方法进行了探讨,在比较二种合成路线的基础上,对适宜的合成途径合成中的关键问题进行了讨论.     

Kinetics of lipid oxidation in the presence of cinnamic acid derivatives

The effects of seven (prenyl‐ and methoxy‐) derivatives of cinnamic acid (0.1 mM) on the kinetics of lipid (sunflower oil triacylglycerols, TGSO) bulk phase oxidation at 80 °C have been compared. Synthesis of prenyl cinnamic acid derivatives: 3‐prenyl‐4‐hydroxy‐cinnamic acid (PHC), 3,5‐diprenyl‐4‐hydroxy‐cinnamic acid (DPHC), 2,2‐di‐methyl‐6‐carboxy‐ethenyl‐2H‐benzopyran (DMCB), 2,2‐dimethyl‐6‐carboxy‐ethenyl‐8‐prenyl‐2H‐benzopyran (DCEPB) present in Brazilian propolis has been performed. The monoprenyl derivative (PHC) has been found to exert a higher antioxidant activity as compared to the diprenyl derivative (DPHC). However, cinnamic acid derivatives DMCB and DCEPB have caused no change in the kinetics of TGSO oxidation. The results obtained have been compared with those on related compounds containing a cinnamic acid moiety as a structural feature, such as 4‐hydroxy‐cinnamic (p‐coumaric), 3‐methoxy‐4‐hydroxy‐cinnamic (ferulic) and 3,5‐dimethoxy‐4‐hydroxy‐cinnamic (sinapic) acids, as well as with data on butylated hydroxytoluene (BHT) and α‐tocopherol (αToc). PHC has shown a stronger antioxidant efficiency than BHT, p‐coumaric and ferulic acid, but a weaker antioxidant efficiency than α‐Toc and sinapic acid. The observed antioxidant effect of DPHC was stronger than that of p‐coumaric and ferulic acids and weaker than that of α‐Toc, BHT and sinapic acid.     

KF/K2CO3/γ-Al2O3催化合成肉桂酸

以苯甲醛和丙二酸为原料,KF/K2CO3/γ-Al2O3为催化剂,经Knoevenagel反应,在无溶剂条件下催化合成了肉桂酸。产品用IR、1HNMR及元素分析进行表征。考察了催化剂用量、苯甲醛与丙二酸摩尔比和反应时间对肉桂酸收率的影响。结果表明:KF/K2CO3/γ-Al2O3具有良好的催化活性,较佳工艺条件为:苯甲醛10.2 mL(10.6 g,0.1 mol),n(苯甲醛)∶n(丙二酸)=1∶1.15,催化剂KF/K2CO3/γ-Al2O3用量2.5 g(含KF4.68 mmol),反应60 min,肉桂酸的平均收率达到92%以上。     

Radical Scavenging Activity of Lipophilized Products from Lipase-Catalyzed Transesterification of Triolein with Cinnamic and Ferulic Acids

Lipase-catalyzed transesterification of triolein with cinnamic and ferulic acids using an immobilized lipase from Candida antarctica (E.C. 3.1.1.3) was conducted to evaluate the antioxidant activity of the lipophilized products as model systems for enhanced protection of unsaturated oil. The lipophilized products were identified using ESI-MS. Free radical scavenging activity was determined using the DPPH radical method. The polarity of the solvents proved important in determining the radical scavenging activity of the substrates. Ferulic acid showed much higher radical scavenging activity than cinnamic acid, which has limited activity. The esterification of cinnamic acid and ferulic acid with triolein resulted in significant increase and decrease in the radical scavenging activity, respectively. These opposite effects were due to the effect of addition of electron-donating alkyl groups on the predominant mechanism of reaction (hydrogen atom transfer or electron transfer) of a species with DPPH. The effect of esterification of cinnamic acid was confirmed using ethyl cinnamate which greatly enhances the radical scavenging activity. Although, compared to the lipophilized cinnamic acid product, the activity was lower. The radical scavenging activity of the main component isolated from lipophilized cinnamic acid product using solid phase extraction, monocinnamoyl dioleoyl glycerol, was as good as the unseparated mixture of lipophilized product. Based on the ratio of a substrate to DPPH concentration, lipophilized ferulic acid was a much more efficient radical scavenger than lipophilized cinnamic acid.     

微生物Mucor sp.转化肉桂酸生成苯乙酮降解途径分析

利用GC-MS检测Mucor sp.转化肉桂酸的产物,对微生物Mucor sp.降解肉桂酸的途径进行了分析。β-苯乙醇首次作为微生物Mucor sp.转化肉桂酸生成苯乙酮的中间体在产物中被检测到。Mucor sp.降解肉桂酸的途径是:在肉桂酸的侧链双键上先发生环氧化反应得到3-苯基-2,3-环氧丙酸,环氧化合物经脱羧、还原开环得到中间体β-苯乙醇,β-苯乙醇经羟基转移和进一步催化氧化生成苯乙酮。     

氯化铁催化合成肉桂酸异丁酯

研究了氯化铁催化下的肉桂酸和异丁醇的酯化反应，得出的优惠条件是，酸醇比为１１０，催化剂用量为０．０９２５ｍｏｌ（对１ｍｏｌ肉桂酸），反应时间３ｈ。在优惠条件下转化率８５．８％。     

Kinetics of Cinnamoyl Glycerol Formation

The esterifications of glycerol with cinnamic acid, 2-methoxy cinnamic acid, and 4-methoxy cinnamic acid were investigated in batch reactions. Conversions of over 50% were achieved for cinnamic acid and 4-methoxy cinnamic acid within 8 h. After 24 h, conversions of over 80% were obtained for cinnamic acid and 4-methoxy cinnamic acid. Conversions of 33 and 40% were observed for 2-methoxy cinnamic acid after 8 and 24 h, respectively. These reactions were modeled by a system of sequential first-order rate expressions. Kinetic parameters were estimated from experimental data fit to the model equations. Disclaimer The use of trade, firm, or corporation names in this publication is for the information and convenience of the reader. Such use does not constitute an official endorsement or approval by the United States Department of Agriculture or the Agricultural Research Service of any product or service to the exclusion of others that may be suitable.     

杂多酸催化合成肉桂酸正丁酯的研究

以钨硅杂多酸为催化剂，通过肉桂酸和正丁醇反应合成肉桂酸正丁酯．实验证明，钨硅杂多酸是合成肉桂酸正丁酯的良好催化剂，在酸醇物质的量比为1：2．0，催化剂用量1．0g／0．05mol肉桂酸，带水剂苯8ml，反应时间为110min条件下，肉桂酸正丁酯的酯化率可达96%．     

钨硅酸催化合成桂酸戊酯的研究

以钨硅酸为催化剂,通过桂酸和戊醇酯化反应合成桂酸戊酯,研究了各有关因素对产品酯化率的影响。实验证明,钨硅酸是合成桂酸戊酯的良好催化剂,在酸醇物质的量比为1∶2.5,催化剂用量为1g/0.05mol桂酸,带水剂苯为7mL,反应时间为1.5h条件下,桂酸戊酯的酯化率可达99.2%。     

桂皮酸苦参碱的合成

目的：合成桂皮酸苦参碱并优化其合成工艺。方法：以苦参碱和桂皮酸为原料合成桂皮酸苦参碱。结果：桂皮酸苦参碱收率达90％,产物的化学结构经TLC、IR、MS等确证。结论：所设计的合成技术简单易行。