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1.
以2-羟基蒎烷-3-酮(1)与氨基乙腈缩合得到的手性酮亚胺(2)为中间体,经去质子化,在Pd(0)催化下与1,4-二氯-2-丁烯(3)发生串联反应,得到光学活性环丙烷衍生物(4),产率约为70%,反应的非对映立体选择性(d.e.)为100%.化合物4经选择性还原后水解,即可制得光学活性2-乙基环丙烷氨基酸,产物的对映体过量(e.e.)为33%.  相似文献   

2.
杨发福  陈远荫 《合成化学》2002,10(2):151-153
研究了在几种反应体系中对叔丁基杯[6]-1,4-冠醚的合成,发现K2CO3/甲苯体系能高选择性地合成目标物,产率比文献报道提高了近一倍。并对反应机理作了初步探讨。  相似文献   

3.
微波辐射下的1,4-二甲基咔唑-9-羧酸的快速合成   总被引:1,自引:0,他引:1  
以DMF为溶剂,在微波辐射下由1,4-二甲基咔唑和相应的溴酯快速合成了两种1,4-二甲基咔唑-9-羧酸化合物,在最佳反应条件下,产率分别为85.2%和83.1%。  相似文献   

4.
报道了以Rh(I)-手性2-(2-吡啶基)-4-羧甲基-1,3-噻唑烷为催化剂,2-氨基芳香酮的不对称硅氢化反应,在常温常压下手性2-氨基-1-芳基乙醇的产率几乎可达定量,产品光学纯度可达80%e.e以上。  相似文献   

5.
N-(取代苯基)-2-(对氯苯氧乙酰基)氨基脲的合成与表征   总被引:2,自引:0,他引:2  
以无机碱为催化剂,用不同的N-(聚代基)三氯乙酰胺与对氯苯氧乙酰肼反应,首次合成了3种新的取代氨基基脲化合物N-(取代苯基)-2-(对氯苯氧乙酰基)氨基脲,产率71%以上。  相似文献   

6.
一锅法合成11-氨基十一酸的研究   总被引:3,自引:1,他引:3  
崔建兰 《合成化学》2002,10(4):374-376
探索了一锅法合成11-氨基十一酸的方法,与分步合成法相比,一锅法具有操作简便、反应条件温和、无需分离中间体、产率较高等特点。并讨论了温度、反应时间、氨比等对一锅法合成产率的影响。  相似文献   

7.
2-(E-2-苯乙烯基)喹啉的合成   总被引:4,自引:1,他引:4  
杨定乔  曾和平  彭柳  吕芬 《合成化学》2002,10(2):154-155,160
以苯甲醛为原料在碱性条件下与丙酮缩合得苄叉丙酮(1),1与邻氨基苯甲醛发生Friedlaender缩合反应得到新的目标产物2-(E-2-苯乙烯基)喹啉(2),产率81%。  相似文献   

8.
Δ6 去饱和酶催化合成γ-亚麻酸   总被引:2,自引:0,他引:2  
报道了含△6去饱和酶的深黄被孢霉菌丝提取物催化亚油酸合成γ-亚麻酸.研究了辅酶、温度、时间等对γ-亚麻酸合成的影响.结果表明,反应温度降低,γ-亚麻酸的产率提高.在10℃以下.γ-亚麻酸的产率达到最大值;苹果酸盐对该反应有明显促进作用.γ-亚麻酸的产率随体系pH增加而增加,且在pH=7~8时产率较高;该反应需在分子氧存在下进行;NADPH,ATP和CoA是该反应的必需辅酶.在优化的反应条件下,γ-亚麻酸的产量达到0.21mg/mL。  相似文献   

9.
报道了含△6去饱和酶的深黄被孢霉菌丝提取物催化亚油酸合成γ-亚麻酸,研究了辅酶,温度,时间等对γ-亚麻酸合成的影响。结果表明,反应温度降低,γ-亚麻酸的产率提高,在10℃以下,γ-亚麻酸的产率达到最大值;苹果酸盐对该反应有明显促进,γ-亚麻酸的产率随体系pH增加而增加。且在pH=7-8时产率较高;该反应需在分子氧存在下进行;NADPH,ATP和CoA是该反应的必需辅酶。在优化的反应条件下,γ-亚麻酸的疸这到.21mg/mL。  相似文献   

10.
首先以2-溴-1-(2,3,4-三甲氧基)苯乙酮,四丁基铵-1H-1,2,4-三唑或咪唑为原料,分别合成了2-(1H-1,2,4-三唑-1-基)-1-(2,3,4-三甲氧基)苯乙酮(Ia)和2-(1H-咪唑0-1-基)-1-(2,3,4-三甲氧基)苯乙酮(Ib)与盐酸羟胺反应生成2-(1H-1,2,4-三唑-1-基)-1-(2,3,4-三甲氧基)苯乙酮肟和1-(1H-咪唑-1-基)-1-(2,3,4三甲氧基)苯乙酮肟,产率为63%-72%,并经元素分析,IR和1H NMR进行了表征。  相似文献   

11.
用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.  相似文献   

12.
In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.  相似文献   

13.
The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.  相似文献   

14.
The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.  相似文献   

15.
KMnO4-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.  相似文献   

16.
The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.  相似文献   

17.
Zhanhui Yang  Shiyi Yang  Jiaxi Xu 《Tetrahedron》2017,73(23):3240-3248
Regiospecific and direct imidation of the methyl C(sp3)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.  相似文献   

18.
19.
《Tetrahedron》2014,70(21):3377-3384
The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.  相似文献   

20.
Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.  相似文献   

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