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total synthesis
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  全合成
     Total Synthesis of (±)-Shegansu B, Gnetuhainin F, (±)-Maackin A and (±)-Cassigarol E
     (±)-Shegansu B,Gnetuhainin F,(±)-Maackin A与(±)-Cassigarol E的全合成
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     Total Synthesis of (±) Cudraflavanone B and (±)-5-O-Methyl Cudraflavanone B
     (±)Cudraflavanone B及(±)-5-O-Methyl Cudraflavanone B的全合成研究
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     Total Synthesis of (±)-19-Norabieta-4(18),8,11,13-tetraen-7-one
     (±)-19-去甲基-4(18),8,11,13-四烯-松香烷-7-酮的全合成
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     Studies on the Total Synthesis of Clavaserine Ⅰ. Synthesis of 3-[(3'R, 5'S)-7'-oxo-1'-aza-4'-oxa-bicyclo [3.2.0] hept-3'-yl]-3-O-benzyl-(2S, 3S)-serine and Its (3'R, 5'R)-epimer from D-glucose
     棒丝氨酸的全合成研究 Ⅰ.从D-葡萄糖合成3-[(3′R,5′S)-7′-氧代-1′-氮杂-4′-氧杂双环[3.2.0]-庚-3′-基]-3-O-苄基-(2S,3S)-丝氨酸及其(3′R,5′R)-差向异构体
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     The Total Synthesis of Acerogenin G and 1,7 Bis (4 hydroxyphenyl) 1,4,6 heptatrien 3 one
     Acerogenin G和1,7-双-(4-羟基苯基)-1,4,6-庚三烯-3-酮的全合成
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  “total synthesis”译为未确定词的双语例句
     TOTAL SYNTHESIS OF 3α,4α-OXIDOAGAROFURAN AND (-)-3β,4α-DIHYDROXY-β-DIHYDROAGAROFURAN
     TOTAL SYNTHESIS OF 3α,4α-OXIDOAGAROFURAN AND (-)-3β,4α-DIHYDROXY-β-DIHYDROAGAROFURAN
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     STUDIES ON THE TOTAL SYNTHESIS OF(-)-(2R, 5S)-2-METHYL-5-HYDROXYMETHYL-δ-VALEROLACTONE
     STUDIES ON THE TOTAL SYNTHESIS OF(-)-(2R,5S)-2-METHYL-5-HYDROXYMETHYL-δ-VALEROLACTONE
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     TOTAL SYNTHESIS OF CURVULARIN-TYPE MACROLIDES 12-OXOCURVULARIN AND CITREOFURAN
     TOTAL SYNTHESIS OF CURVULARIN-TYPE MACROLIDES 12-OXOCURVULARIN AND CITREOFURAN
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     STUDIES ON THE PRENYLFLAVONOIDS PART Ⅹ:THE TOTAL SYNTHESIS OF ANTIARONE-C AND ANTIARONE-H
     STUDIES ON THE PRENYLFLAVONOIDS PART Ⅹ:THE TOTAL SYNTHESIS OF ANTIARONE-C AND ANTIARONE-H
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     STUDIES ON THE PRENYLFLAVONOIDS PART XI: THE TOTAL SYNTHESIS OF(±)-AMORISIN AND(±)-SIGMOIDIN-B
     STUDIES ON THE PRENYLFLAVONOIDS PART XI: THE TOTAL SYNTHESIS OF (±)-AMORISIN AND (±)-SIGMOIDIN-B
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  相似匹配句对
     Total Synthesis of Irisquinone
     马蔺子甲素的全合成
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     Total Synthesis of Anisodine
     樟柳碱的全合成(英文)
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     Synthesis of p
     对氯苯甲醛的合成
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  total synthesis
An optimized procedure was suggested for synthesis of I and Ia using an Anatech robotic system; the total synthesis time is 45-48 min.
      
[18F]FET was prepared with a high radiochemical purity (>amp;gt;95%); the total synthesis time, including HPLC purification, was 60 min, and the unoptimized radiochemical yield (corrected for the radioactive decay) was about 20%.
      
A total synthesis of 8α analogues of steroid estrogens with fluorine in position 2 was achieved.
      
The total synthesis of α-(4'-benzoylphenyl)-α-methyl propionic acid was monitored by thin-layer chromatography.
      
Total synthesis of human Β-endorphin gene has been designed for the expression in bacterial system.
      
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In the present paper, the total synthesis of liensinine, an alkaloid of embryo loti,Nelumbo nucifera Geartn., was described. 1-(3'-Bromo-4'-benzyloxy)benzy1-2-methyl-6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline (Ⅷ) and 1-(4'-benzyloxy)benzyl-2-methyl-6-methoxy-7-hydroxy-1,2,3,4-tetrahydroisoquinoline (ⅩⅤ),the two key intermediates,have firstly been synthesized. N-β-(3,4-dimethoxy)phenylethyl amine was condensed with 3-bromo-4-benzyloxy-phenylacetic acid to give the corresponding amide(Ⅳ).Amide (Ⅸ) was...

In the present paper, the total synthesis of liensinine, an alkaloid of embryo loti,Nelumbo nucifera Geartn., was described. 1-(3'-Bromo-4'-benzyloxy)benzy1-2-methyl-6,7-dimethoxy-1,2,3,4-tetrahydroisoquinoline (Ⅷ) and 1-(4'-benzyloxy)benzyl-2-methyl-6-methoxy-7-hydroxy-1,2,3,4-tetrahydroisoquinoline (ⅩⅤ),the two key intermediates,have firstly been synthesized. N-β-(3,4-dimethoxy)phenylethyl amine was condensed with 3-bromo-4-benzyloxy-phenylacetic acid to give the corresponding amide(Ⅳ).Amide (Ⅸ) was converted to the acetyl derivative(Ⅹ). By the Bischler-Nipierlski reaction,compounds(Ⅳ)and(Ⅹ)underwent cyclodehydration to give the corresponding 3,4-dihydroisoquinoline derivatives(Ⅴ)and(Ⅺ).Reduction of the latters with potassium borohydride or sodium borohydride afforded 1- (3'-bromo-4'-benzyloxy) benzyl-6,7-di-methoxy-1,2,3,4-tetrahydroisoquinoline(Ⅵ) and 1-(4'-benzyloxy)benzyl-6-methoxy-7- acetoxy-1,2,3,4-tetrahydroisoquinoline (ⅩⅢ), which were then N-methylated to give Ⅷ and ⅪⅤ respectively.Compound ⅪⅤ was hydrolyzed to afford at last ⅩⅤ. Compound Ⅷ and ⅩⅤ were also prepared by reducing the methiodides Ⅶ and Ⅻ obtained by treatment of compound Ⅴ and Ⅺ with methyl iodide. Secondly the compounds Ⅵ and Ⅷ were resolved into their optical antipodes with satisfactory yield with the aid of (+)-and(-)-DPT-tartaric acid.After N-methyla-tion both D-(-)-Ⅵ and L-(+)-Ⅵ afforded oily D-(-)-Ⅷ and L-(+)-Ⅷ characterized as their crystalline oxalates.D-(+)-ⅩⅢ and L-(-)-ⅩⅢ were methylated and followed by alkaline hydrolysis to give D-(-)-ⅩⅤ and L-(+)-ⅩⅤ respectively. Finally, while D-(-)-Ⅷ and D-(-)-ⅩⅤ were subjected to Ullmann reaction in pyridine in the presence of copper powder and potassium carbonate, there was obtained an oily substance by employing chromatography on alumina. The oily substance was then hydrolyzed to a yellowish amorphorus solid which was converted to crystalline perchlorate identical with natural liensinine perchlorate in all respects.(±)-Liensinine was also synthesized by the condensation of (±)-Ⅷ and (±)-XV in the same condition.

本文报导了莲心碱(Ⅰ)全合成的研究。 (1)合成了1-(3′-溴-4′-苄氧基)苄基-2-甲基-6,7-二甲氧基-1,2,3,4-四氢异喹啉(Ⅷ)和1-(4′-苄氧基)苄基-2-甲基-6-甲氧基7-羟基-1,2,3,4-四氢异喹啉(XV).(2)1-(3′-溴-4′-苄氧基)苄基-6,7-二甲氧基-1,2,3,4-四氢异喹啉(Ⅵ)和1-(4′-苄氧基)苄基-6-甲氧基-7-乙酰氧基-1,2,3,4-四氢异喹啉(ⅩⅢ)借d-和1-DPT-酒石酸各自拆分为其对映体。D-(-)-Ⅵ和L-(+)-Ⅵ以甲酸和甲醛甲基化分别生成D-(-)-Ⅷ和L-(+)-Ⅷ。D-(+)-;ⅩⅢ和L-(-)-ⅩⅢ经N-甲基化后再进行水解卽得D-(-)-ⅩⅤ和L-(+)+ⅩⅤ。(3)D-(-)-Ⅷ和D-(-)-ⅩⅤ在吡啶中有铜粉和碳酸钾存在下进行Ullmann反应,反应物经氧化鋁柱层析可分得一油状物,此油状物经盐酸水解得黄色无定形固体,后者与过氯酸生成过氯酸盐结晶,其理化性质均与天然莲心碱过氯酸盐相同。(±)-Ⅷ和(±)-ⅩⅤ在相似的条件下缩合则生成(±)-莲心碱。

Dodecapeptide ester Ⅰ has been saponified to give a protected C-terminal dodecapeptide (Ⅱ) of the A-Chain of insulin. Further experiments showed that the saponification of ester Ⅰ under various conditions yielded preparations of dodecapeptide Ⅱ varying somewhat in melting points and solubility. These saponification products have been used for the partial synthesis of bovine insulin and all the crude hormone products obtained showed biological activity of 1—4% of natural insulin in mouse convulsion test. In order...

Dodecapeptide ester Ⅰ has been saponified to give a protected C-terminal dodecapeptide (Ⅱ) of the A-Chain of insulin. Further experiments showed that the saponification of ester Ⅰ under various conditions yielded preparations of dodecapeptide Ⅱ varying somewhat in melting points and solubility. These saponification products have been used for the partial synthesis of bovine insulin and all the crude hormone products obtained showed biological activity of 1—4% of natural insulin in mouse convulsion test. In order to avoid the saponification dodecapeptide Ⅱ has been directly synthesized by two alternative routes. By route 1, the known tetrapeptide Ⅲ was first converted into its hydrazide (Ⅳ), which was then coupled by the azide method with pentapeptide V_b to form nonapepfide Ⅵ (C_(66)H_(86)N_(12)O_(19)S·2H_2O, m.p. 235—236° (decomp.), [α]_D~(15)—44° (c 1.0, DMF)). Nonapeptide Ⅵ was decarbobenzoxylated and combined with the known tripeptide hydrazide Ⅶ through the azide method to give dodecapeptide Ⅱ(C_(84)H_(111)N_(15)O_(23)S_2·2H_2O, m.p. 246—248°, [α]_D~(15)—34° (c 1.0, HCOOH)). Pentapeptide V_b was prepared from pentapeptide V which was obtained by the following ways: (1) The known dipeptide ⅩⅢ was decarbobenzoxylated and the N-deblocked product was combined with dipeptide hydrazide ⅩⅣ by the azide method to form tetrapeptide XV (C_(35)H_(40)N_6O_(10)S·H_2O, m.p. 191—193°, [α]_D~(21)-41° (c 1.0, DMF)). The same product has also been synthesized by coupling N-carbobenzoxy-L-asparagine p-nitrophenyl ester with N-deblocked tripeptide ⅩⅧ. Compound ⅩⅧ was in turn prepared from the condensation of N-carbobenzoxy-L-tyrosyl hydrazide with N-deblocked dipeptide ⅩⅢ (m.p. 188—190°, [α]_D~(30)-34° (c 1.0, DMF)). Tetrapeptide ⅩⅣ was further decarbobenzoxylated and the resulting product was condensed with α-p-nitrophenyl-γ-tert-butyl N-carbobenzoxy-L-glutamate (ⅩⅦ) to yield pentapeptide Ⅴ (C_(44)H_(55)N_7O_(13)S·H_2O, m.p. 185—186°, [α]_D~(22)-37° (c 2.0, DMF)). Both compounds ⅩⅧ and ⅩⅤ have been prepared by another method. (2) N-deblocked dipeptide ⅩⅥ was first coupled with ⅩⅦ to give tripeptide ⅩⅪ (m.p. 179—180°, [α]_D~(32)+7° (c 1.0, DMF)), which was then converted into its hydrazide ⅩⅫ (m.p. 219—220°,[α]_D~(32)—16.5° (c 1.0, DMF)). Hydrazide ⅩⅫ was finally condensed by the azide method with dipeptide ⅩⅢ to yield pentapeptide V. It seems that way (1) led to better overall yield and higher quality of the pentapeptide. By route 2, dodecapeptide Ⅱ was synthesized by condensing heptapeptide hydrazide ⅩⅩⅦ with pentapeptide V_b through the azide method. Hydrazide ⅩⅩⅦ (C_(52)H_(74)N_(10)O_(12)S·H_δO, m.p. 253—254° (decomp.), [α]_D~(26)-36° (c 0.93, HCOOH)) was prepared from heptapeptide ester ⅩⅩⅥ. Ester ⅩⅩⅥ was synthesized by two alternative methods. In one of these methods tripeptide hydrazide Ⅶ was transformed into its azide and condensed with decarbobenzoxylated dipeptide ester ⅩⅩⅢ to form pentapeptide ester ⅩⅩⅣ (C_(43)H_(57)N_5O_(10)S·H_2O, m.p. 220—222°,[α]_D~(15)-21° (c 1.0, DMF)), which was then converted into its hydrazide ⅩⅩⅤ and finally coupled through the azide method with N-deblocked dipeptide Ⅹ to give heptapeptide ester ⅩⅩⅥ (C_(53)H_(74)N_8O_(13)S·H_2O, m.p. 249—250° (decomp.), [α]_D~(15)-34° (c 1.0, DMF)). In the other method, ester ⅩⅩⅥ was obtained from tripeptide hydrazide Ⅶ and N-deblocked tetrapeptide Ⅲ by the azide method. All synthetic peptide intermediates have been subjected to elementary analyses, as well as paper chromatographic and paper electrophoretic examinations, and dodecapeptide Ⅱ has been analysed for its amino acid composition. The results showed that all synthetic peptides are chemically pure and homogeneous. Dodecapeptide Ⅱ prepared by the above routes has higher melting point and levorotatory power than that obtained by the saponification of ester Ⅰ. It has been used for the partial as well as total synthesis of crystalline bovine insulin.

已知合成的胰岛素A链羧端带保护基的十二肽酯Ⅰ在不同条件下皂化,得十二肽Ⅱ,其物理性质略有差异,经制成牛胰岛素A链井进一步制成半合成牛胰岛素粗产物后,其生物活力相当于天然胰岛素的1—4%。根据二条不同的路线直接合成了带保护基的胰岛素A链羧端十二肽Ⅱ,路线一:由已知的四肽Ⅲ制成其酰肼衍生物,再转变为相应的迭氮化物后与脱N-苄氧羰基和γ-叔丁基的五肽Ⅴ(即Vb)缩合成九肽Ⅵ,Ⅵ经脱除N-保护基后与已知的三肽酰肼Ⅶ以迭氮化物法缩合郎得十二肽Ⅱ.路线二:三肽酰肼Ⅶ先制成迭氮化物再与脱N-保护基的已知二肽酯ⅩⅩⅢ反应成五肽酯ⅩⅩⅣ,再经肼解得五肽酰肼ⅩⅩⅤ,然后按迭氮化物法与脱苄氧羰基的二肽Ⅹ缩合成七肽酯ⅩⅩⅥ,再肼解得七肽酰肼ⅩⅩⅦ,最后通过迭氮化物法与五肽V_b缩合,亦得相同的十二肽Ⅱ.由这两种方法直接合成的十二肽Ⅱ,其质量较皂化所得为优,并已用于牛胰岛素A链的合成与结晶牛胰岛素的半合成和全合成。五肽Ⅴ和七肽ⅩⅩⅥ都曾各按二条不同的路线合成,而得到相同的产物,本文报导的合成肽段均经分析证明为化学纯的均一物质。

Chairman Mao taught us, "One should seriously sum up one's experience." Looking back at the experiences of our own and of others in the past decade or so on the total synthesis of proteins and polypeptides, we have analyzed the inherent contradictions of the two alternative routes of synthesis on the basis of the dialectical viewpoint of "one divides into two". Either the solid phase or the solution synthesis is fraught with difficulties when the target exceeds 100 amino acids. A new synthetic...

Chairman Mao taught us, "One should seriously sum up one's experience." Looking back at the experiences of our own and of others in the past decade or so on the total synthesis of proteins and polypeptides, we have analyzed the inherent contradictions of the two alternative routes of synthesis on the basis of the dialectical viewpoint of "one divides into two". Either the solid phase or the solution synthesis is fraught with difficulties when the target exceeds 100 amino acids. A new synthetic strategy was developed which we believe could resolve the contradictions inherent in the synthesis of large peptides-the solid phase stepwise condensation of peptide fragments instead of amino acids. Following repeated practice guided by the spirit of independence and self-reliance, we succeeded in synthesizing first of all a new supporting medium which provisionally met our requirements. We shall describe in the present paper the successful total synthesis of the nonacosapeptide glucagon using this supporting medium. Four peptide fragments (5, 6, 9, 6), synthesized with the aid of classical methods, were coupled stepwise to a resin-bound tripeptide, with an efficiency of over 95% for each step. After treatment with hydrogen fluoride and purification twice by means of column chromatography, rhombic dodecahedral crystals of glucagon could be obtained which were identical with natural products in respect of amino acid composition, chromatographic and discelectrophoretic behaviour, etc. The overall yield was about 17%. In view of the characteristic abundance in glucagon of various kinds of functional groups which impart unfavourable obstacles to the course of synthesis, this relatively high yield and the ease with which crystalline products could be obtained testify to the potential of the new technique in the eventual total synthesis of larger proteins.

遵照毛主席关于“要认真总结经验”的教导,作者在回顾十年来多肽合成发展过程的基础上,运用一分为二的唯物辩证观点分析了目前已有的两类合成方法都难以合成含100个氨基酸残基以上的大蛋白质的内在矛盾,指出了可能解决矛盾的途径之一,一个新的合成方案——片段固相缩合法。在“独立自主、自力更生”方针的指引下,通过反复实践,我们合成了初步满足新方法所需要的新材料——表层树脂。本文报导合成胰高血糖素(29肽)的结果,目的是对新方法进行一次考验:先将用经典法合成的四个肽片段(5,6,9,6)在三肽树脂上依次进行缩合,每次缩合率皆达95%以上,全合成以后经过氟化氢处理,两次柱分离纯化,便可获得氨基酸组成、层析及碟状电泳等物化行为与天然品相同的,具有高效增血糖活力的胰高血糖素结晶——正交十二面体。全过程总得率可达17%。根据在胰高血糖素的组成中含有侧链功能团氨基酸较多的特点,在虽然给人工合成过程带来不利影响的情况下仍能获得较高缩合率及通过简单分离即能纯化结晶的结果,说明这一方法有可能为人工合成具有严格结构的较大蛋白质提供一条发展途径。

 
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