新型吡啶基吡唑酰胺类化合物的合成

以2,3-二氯吡啶为起始原料,经过肼解、与马来酸二乙酯成环、卤代、氧化和水解得到关键中间体吡啶基吡唑甲酸,然后与二氯亚砜反应生成甲酰氯,最后与各种环氨作用生成吡啶基吡唑甲酰胺类化合物。     

3-羰基-10-去甲基-12-甲氧基-13-甲基罗汉松烷的全合成

以1,3-环己二酮为原料,经过甲基化反应和羰基保护构筑了A环合成子(5)。以邻甲基苯甲醚为原料,对位溴代、与环氧乙烷加成和进一步溴代等反应合成了C环合成子(9)。化合物5与9的格氏试剂偶联和关环反应完成目标产物3-羰基-10-去甲基-12-甲氧基-13-甲基罗汉松烷(11)的全合成。各中间体及目标产物结构均经红外光谱、核磁、质谱等表征,结果表明,成功实现了目标产物的合成。     

双环笼状四配位硅的合成及其结构表征

研究了以SiO₂为原料低温合成高反应活性的五配位硅酸酯, 并与1-氧代-1-磷杂-2,6,7-三氧杂双环[2.2.2]-4-氯甲基辛烷反应合成出具有对称结构的双环笼状四配位硅, 通过红外光谱、¹³C和²⁹Si固体核磁共振、质谱等测试手段确定了其结构. 热分析结果表明, 双环笼状四配位硅在700 ℃的失重仅为19.98%, 且炭层呈密实片层状, 说明目标产物具有优异的热稳定性和成炭性质.     

树枝状偶氮液晶高分子(PAMAM-MMAZO)的合成及表征

树枝状偶氮液晶高分子(PAMAM-MMAZO)的合成及表征;树枝状聚酰胺-胺;树枝状偶氮液晶;表面修饰;液晶性     

Synthesis of the metabolites of 4-(2-methyl-1H-imidazol-1-yl)-2,2-diphenylbutanamide (KRP-197/ONO-8025)

We synthesized the six presumed metabolites (2--7) of 4-(2-methyl-1H-imidazol-1-yl)-2,2-diphenylbutanamide [KRP-197/ONO-8025, 1], a urinary incontinence therapeutic agent, in order to confirm the structures of the metabolites. Metabolite (2) was synthesized via glucuronidaion of compound (1) and methyl 2,3,4-tri-O-benzoyl-1-methanesulfonyl-alpha-D-glucopyranuronate. Metabolite (3) was synthesized via 3-(tert-butoxycarbonyl)-2-methyl-1,3-imidazolidine-4,5-dione. Metabolites (4--7) were synthesized via 4-amino-2-diphenylbutanamide, respectively. The structures of the metabolites (2--7) in humans were identified by means of synthesis of the authentic compounds.     

N-(2-氨基苯基)-2-喹唑啉酮乙酰胺盐酸盐的合成

本文通过2-溴-N-(2-硝基苯)乙酰胺和取代的喹唑啉酮在NaH催化下发生亲核取代反应,再经过氢化、酸化合成了4个新型常山碱类抗球虫药物-N-(2-氨基苯基)-2-喹唑啉酮乙酰胺盐酸盐(1∶1)。其中,2-溴-N-(2-硝基苯)乙酰胺通过溴乙酰氯与邻硝基苯胺反应制备,取代的喹唑啉酮使用取代的邻氨基苯甲酸与甲酰胺反应合成。所有目标化合物的结构均经1H NMR,IR和HRMS等方法确证。     

卡托普利合成工艺改进及有关物质合成

以(2S)-1-(3-巯基-2-甲基-1-氧代丙基)-L-脯氨酸为起始物料,经水解、盐析、精制合成了卡托普利,总收率85%,纯度99.72%,单杂小于0.1%。基于该工艺合成了卡托普利的5种杂质,纯度均大于95.0%,结构经1H NMR,13C NMR和HR-MS(ESI)确证。     

Synthesis and properties of aminomethoxy derivatives of 1-(butylsulfanyl)pentane

New aminomethoxy derivatives of 1-(butylsulfanyl)pentane have been synthesized. The structure of the synthesized compounds was studied by elemental analysis, IR and ¹Н NMR spectroscopy, and mass spectrometry. Some specimens of the synthesized compounds were tested as antimicrobial additives to lubricant oil, and as aseptic compounds against bacteria and fungi.     

Synthesis of methyleneoxyamino derivatives of 1-butylthioheptane

The possibility of synthesizing new methyleneoxyamino derivatives of 1-butylthioheptane was investigated. The structure of the synthesized compounds was proved by elemental analysis and IR and ¹H NMR spectroscopy. Some representatives of the synthesized compounds were tested as antimicrobial lubricant additives, and also as antiseptic materials against bacteria and funguses.     

Studies on Agarofurans IV. The Synthesis of 4-Substitutioned Agarofurans

A new synthetic route for α-agarofuran(1b) is described. Several agarofuran derivatives were synthesized in similar way. Derivative 1d was also synthesized in a novel way, in which the substitution at C-4 was performed quantitatively. An ideal condition for cyclization of diol 7 to agarofuran (1) was found.     

两种氮杂环丁烷类药物中间体的合成

1-二苯甲基-3-羟基氮杂环丁烷(1)经过对甲苯磺酰氯取代、叠氮化及还原反应合成了药物中间体--1-二苯甲基-3-氨基氮杂环丁烷(4);1经过氧化、氰基化与还原反应合成了1-二苯甲基-3-羟基-3-氨甲基氮杂环丁烷(8).4和8的结构经1H NMR表征.     

Synthesis of cis- and trans-5,8-dihydroxy-5,6,7,8-tetrahydro-1,4-naphthoquinone

Cis- and trans-5,8-dihydroxy-5,6,7,8-tetrahydro-1,4-naphthoquinone (1a, 1b) were for the first time synthesized from 5,8-dihydroxy-1,4-naphthoquinone (naphthazazine) (6) as a starting material and racemic triol (3) was first synthesized from 7. The configuration of 1a was determined by X-ray analysis.     

盐酸奈法唑酮的合成

盐酸奈法唑酮是一类新型抗抑郁药.先用间氯苯胺与二乙醇胺环化合成1-(3-氯苯基)哌嗪,再与1-溴-3-氯丙烷反应制得1-(3-氯丙基)-4-(3-氯苯基)哌嗪盐酸盐,最后与5-乙基-4-(2-苯氧乙基)-1,2,4-三唑-3-酮反应得到盐酸奈法唑酮.产物结构经IR,MS,1H NMR及13C NMR确证.     

1,1'-不同酰基二茂铁衍生物的合成和波谱研究

以乙酰基二茂铁和相应的乙酰氯在三氯化铝存在下在 流室温条件下合成了不对称二乙酰基二茂铁衍生物; 1-乙酰基-1'-卤素取代苯甲酰基二茂铁, 除了获得预期产品以外, 当反应在 流温度下进行时, 还得到1,3-二(二茂铁基)-丁烯-2-酮-1, 用同样方法还合成了1-乙酰基-1'-棕榈酰二茂铁和1-苯甲酰-1'-棕榈酰基二茂铁.     

Synthesis, Crystal Structure and Biological Activities of 2- （4-Fluorophenyl） -2-oxo-1-（1H-1,2,4-triazol-1-yl） ethyl morpholine-4-carbodithioate

The title compound, 2-（ 4-fluorophenyl ） -2-oxo-1-（ 1H-1, 2,4-triazol-1-yl ） ethyl morpholine-4-carbodithioate, was synthesized and its structure was confirmed by means of IR, MS, 1 H 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 possesses some biological activities.     

Total synthesis of (+)-pederin. 2. Stereocontrolled synthesis of (+)-benzoylselenopederic acid and total synthesis of (+)-pederin

(+)-Benzoylselenopederic acid (1), a left half of (+)-pederin (3), was synthesized stereoselectively based on the Zn(BH₄)₂ reduction and total synthesis of (+)-pederin (3) was accomplished from 1 and the previously synthesized 2.     

Synthesis, Crystal Structure and Biological Activities of N＇ - （ 4-Methoxybenzylidene ） -2- （ 1H-1, 2,4- triazol-1-yl） acetohydrazide

The title compound, N‘-( 4-methoxybenzylidene ) -2-( IH-1, 2,4-triazol-1-yl ) acetohydrazide, was synthesized and its structure was confirmed by means of 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 shows that the synthesized compound has a low antifungal activity.     

新型含1,2,3-三氮唑的染料木素糖缀合物的合成

以染料木素为起始原料,经两步反应制得中间体7-O-炔丙基染料木素(3);以CuI为催化剂,3与叠氮乙酰基糖经Click反应合成了7-O-［1-(2,3,4,6-四-O-乙酰基-β-D-糖苷)1H-1,2,3-三氮唑-4-甲基］-染料木素(5a~5c); 5a~5c经去乙酰基制得三种含1,2,3-三氮唑的氮苷染料木素糖缀合物(6a~6c)。3, 5和6均为新化合物,其结构经¹H NMR, ¹³C NMR和HR-MS表征。     

含氨基的金刚烷桥头二取代化合物合成研究

采用金刚烷甲酸为原料,经溴代、叠氮化、库尔提斯重排、水解等四步反应合成了3-氨基-1-金刚烷醇(糖尿病药物中间体),总收率为34%;以金刚烷甲酸为原料,在无需卤素取代下,通过里特反应、水解反应合成了3-氨基-1-金刚烷甲酸盐酸盐(抗肿瘤药物中间体),总收率为73%.采用元素分析、红外光谱、质谱、核磁共振谱等手段对两种产物的进行了结构鉴定,分别提出了可能的反应机理.     

间叔丁基苯乙醚的合成研究

通过两条路线合成了生产新型农药乙螨唑的关键中间体间叔丁基苯乙醚。其一以叔丁基苯为原料,通过溴代、硝化、还原(脱卤素)、重氮化和乙醚化反应得到目标化合物;另一采用对氨基叔丁基苯为原料,通过乙酰化、溴代、脱乙酰化、重氮化去氨基和乙醚化反应得到目标化合物。两条路线的总收率都较高,分别为45%和63%。所得产品中未检测到异构体对叔丁基苯乙醚,质量好,纯度高。其中路线一原料便宜,操作简单,更适合进一步工业化放大生产。合成路线中的有机中间体和目标化合物的化学结构通过MS和NMR进行确证。