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建立了利托那韦的合成新方法。N-{N-甲基-N-[(2-异丙基-4-噻唑基)甲基]氨基羰基}-L-缬氨酸(1)与(2S,3S,5S)-5-氨基-2-{N-[(5-噻唑基)-甲氧羰基]氨基}-1,6-二苯基-3-羟基己烷在3-(二乙氧基磷酰氧基)-1,2,3-苯并三嗪-4-酮催化下于室温经缩合反应合成了利托那韦,其结构经1H NMR,13C NMR,MS和元素分析确证。在最佳反应条件[1 0.2 mol,DEPBT 0.25 mmol,二氯甲烷为溶剂,三乙胺为缚酸剂,于室温反应过夜]下,收率72.6%。 相似文献
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以7-甲氧基-1-萘满酮为原料,经Wittig反应、去甲基化、烯醇互变和Jones氧化反应等制得关键中间体7-甲氧基-1,2,3,4-四氢化萘-1-羧酸(4); 4-异丙基苯胺和4-(二甲基胺基)苯甲醛经过还原胺化反应得(E)-4-{[(4-异丙基苯基)亚胺基]甲基}-N,N-二甲基苯胺(6); 4转化为相应的酰氯后与6反应合成N-[4-(二甲基氨基)苄基]-N-(4-异丙基苯基)-7-甲氧基-1,2,3,4-四氢化萘-1-甲酰胺(W-54011),总收率24%,其结构经1H NMR, 13C NMR和HR-MS(ESI)表征。
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José Fuentes Mota Fernández José M. García Carmen Ortiz Mellet Pradera Adrián M. Angeles Tomasa Cuevas Lorite 《Journal of carbohydrate chemistry》2013,32(6):837-851
ABSTRACT The syntheses of N-hetaryl (thiazole-2-yl, 2-thiazoline-2-yl, 4,4-diphenyloxazoline-2-yl, cis-3a,4,5,6,7,7a-hexahydrobenzoxazole-2-yl)-N′-(2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl) thioureas (1a-1d), N-hetaryl (2-thiazoline-2-yl, 4,4-diphenyloxazoline-2-yl)-N′-(2,3,4,6-tetra-O-benzoyl-β-D-galactopyranosyl) thioureas (2b, 2c) and 1,2,3,4,6-tetra-O-acetyl-2-deoxy-2-[3-(4′, 4′-diphenyl-2′-y1) thioureido]-β-D-glucopyranose (3c) are described. The structures and conformational properties of prepared compounds are based on analytical and spectroscopic (UV, IR, NMR and MS) data. 相似文献
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SU Zhong min ** CHEN Li hua WU Li xin XU Hong bin ZHU Dong xia WANG Rong shun . The Chemistry Department Functional Material Institute Northeast Normal University Changchun P. R. China . Institute of T 《高等学校化学研究》2002,18(3)
IntroductionSince C. W. Tang firstly reported theelectroluminescence of 8- hydroxyquinolinealuminium[1] ,much attention has been paid to themetal complexes as electro- luminescent materials.Based on a series of experimental data,it has beenknown that the electroluminescence of metalcomplexes with heterocyclic ligands containing Nand O elements mainly results from the tripletstatetransition.For some transitional metal complexes,there exist the transitions from metal to ligand( MLCT) at thei… 相似文献
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Seung Young Lee Kyeong Wan Woo Chung Sub Kim Dong Ung Lee Kang Ro Lee 《Helvetica chimica acta》2013,96(2):320-325
Three new furofuran lignans, (+)‐4,4′‐O‐diangeloylpinoresinol ( 1 ), (+)‐4,4′‐O‐diangeloylmedioresinol ( 2 ), and (+)‐4,4′‐O‐diangeloylsyringaresinol ( 3 ), together with the known compound (+)‐syringaresinol, were isolated from the MeOH extract of Rudbeckia laciniata. The structure elucidation of these compounds were based on 1D‐ and 2D‐NMR, and HR‐ESI‐MS data. The additional structural evidence was obtained from alkaline hydrolysis of the compounds. 相似文献
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The title compound, N-(4-methyl-6-oxo-1,6-dihydro-pyrimidin-2-yl)-N′-(2-trifluoromethyl-phenyl)-guanidine, was synthesized and its structure was confirmed by using IR, MS, 1H NMR, and elemental analysis. The single crystal structure of the title compound was determined by X-ray diffraction. The preliminary biological test showed that the synthesized compound has a weak herbicidal activity. 相似文献
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The metabolism of the potent antiarrythmic drug amiodarone (AMI; 1 ) has yet not been fully investigated. Recently, in vitro experiments revealed that in rabbit‐liver microsomes, AMI ( 1 ) and its main metabolite MDEA ( 2 ) were biotransformed to the hydroxylated derivatives 3′‐OH‐AMI ( 3 ) and 3′‐OH‐MDEA ( 4 ), respectively. To establish the chemical structure of 3 and 4 , we developed a total synthesis of these two metabolites of AMI ( 1 ). 1H‐ and 13C‐NMR Signal assignment from HSQC and HMBC 2D NMR data of synthesized 4 showed that the proposed structure of metabolite 4 is correct. Even the structure of 3 was found to be correct by comparing its HPLC/MS‐MS/MS with the data described earlier. 相似文献
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A Practical Synthesis of 3′-Thioguanosine and of Its 3′-Phosphoramidothioite (a Thiophosphoramidite)
Starting from guanosine, an efficient method for the synthesis of 3′-thioguanosine (see 13 ) and of its 3′-phosphoramidothioite (see 23 ), suitable for automated incorporation into oligonucleotides, was developed. Reaction of 5′-N2-protected guanosine with 2-acetoxyisobutyryl bromide afforded stereoselectively the 2′-O-acetyl-3′-bromo-β-D -xylofuranosyl derivative 3 , which was converted to a 7 : 3 mixture of the S-acyl ribofuranosyl intermediates 5 or 6 and the 3′,4′-unsaturated by-product 4 . The S-acylated nucleosides 5 and 6 were then converted in three steps to 5′-O-(4,4′-dimethoxytrityl)-3′-S-(pyridin-2-ylthio)-3′-thioguanosine ( 11 ), which served as a common intermediate for the preparation of free 3′-thionucleoside 13 and 3′-thionucleoside 3′-phosphoramidothioite 23 . 相似文献