醋氯芬酸的合成

双氯芬酸钠与氯乙酸叔丁酯经酯化、水解反应制得非甾体抗炎药醋氯芬酸,收率82%.     

甜菜碱合成新工艺的研究

报道了合成甜菜碱的新工艺。该法通过氢氧化钙和氯乙酸的中和,氯乙酸钙的三甲胺化两步反应,最后提纯分离制取甜菜碱,产品甜菜碱含量达到（98±1）%。     

盐酸阿洛司琼的合成工艺改进

据文献报道，以3-甲氧甲酰基-2，4-二氧哌啶钠盐（2）为原料，采用两条不同的合成路线，成功地制备了盐酸阿洛司琼（alosetron，1）。路线一以化合物2与1-甲基-1-苯肼硫酸盐缩合得到5，6-二氢-4-(2-甲基-2-苯肼)-2(1H)-吡啶酮（3），再经环合、对接制得盐酸阿洛司琼，总收率为10%。路线二以化合物2经脱竣制得2，4-哌啶二酮（5），与1-甲基-1-苯肼缩合制得3，再经环合、对接制得盐酸阿洛司琼，总收率为23.7%。经IR、UV、^1H-NMR、^13C-NMR及MS测试确证目标化合物结构。     

盐酸甜菜碱在大鼠体内药物代谢动力学及分布

盐酸甜菜碱在大鼠体内药物代谢动力学及分布王桂芳１李伟陈颖莉张艳秋曲淑岩（吉林省中医中药研究院，长春１３００２１）用薄层扫描定量法研究了盐酸甜菜碱在大鼠体内的代谢过程，并测定甜菜碱的血药浓度．盐酸甜菜碱４００ｍｇｋｇ－１ｉｖ后，血药浓度时间曲线拟合符合...     

盐酸利莫那班的合成

对氯苯丙酮经硅烷化制得烯醇硅醚，与草酰氯单乙酯缩合得到α，γ-二酮酸酯，再经成腙、环合、水解、酰胺化和成盐等反应制得盐酸利莫那班，总收率约46％。     

盐到金刚乙胺的合成

以金刚烷为起始原料，经溴化、乙酰化、甲酰胺加成和水解反应，制得盐酸金刚乙胺，总收率３１．５％。     

盐酸加巴喷丁的合成

环己酮与乙腈经Knoevenagel反应、Michael加成反应、Pd-C催化氢化还原和水解反应制得2-羟基-2-氮杂螺[4．5]癸烷-3-酮，再经Raney Ni催化氢化还原和水解、成盐制得抗癫痫药盐酸加巴喷丁，总收率14％。     

盐酸拓扑替康的合成

喜树碱经双氧水氧化、光照重排制得10-羟基喜树碱,继经Mannich反应制得拓扑替康,通入HCl成盐得到盐酸拓扑替康,总收率约30%.     

盐酸二苯美仑合成工艺研究

以苄基氯为起始原料，经5步反应制得盐酸二苯美仑，总收率56.9%，具有反应条件温和、原料价廉易得等优点。     

雷尼替丁枸橼酸铋的合成及其表征

以盐酸雷尼替丁为原料,经碱化制得雷尼替丁（碱基）,再与枸橼酸铋反应制得消化性溃疡治疗药－雷尼替丁枸橼酸铋。经元素分析、红外光谱、核磁共振谱、质谱等确证了结构。     

羧甲淀粉钠中氯乙酸残留对马来酸氯苯那敏稳定性的影响

目的探讨羧甲淀粉钠中残留的氯乙酸对马来酸氯苯那敏稳定性的影响。方法测定不同存放条件下羧甲淀粉钠中氯乙酸残留量,以及以此制备的马来酸氯苯那敏制剂中主成分、最大杂质、总杂质含量,考察羧甲淀粉钠中氯乙酸残留与马来酸氯苯那敏降解程度间的相关性。结果各批样品均有不同程度的氯乙酸残留,近20%的样品氯乙酸残留超过0.2%,最高达1.68%。马来酸氯苯那敏对照品在20℃与40℃条件下存放均稳定,无明显杂质产生;相同存放条件下,马来酸氯苯那敏的降解速率随羧甲淀粉钠中氯乙酸含量的增大而提高;氯乙酸含量相同的羧甲淀粉钠样品的放置温度越高,马来酸氯苯那敏的降解速率越快。结论羧甲淀粉钠中氯乙酸对马来酸氯苯那敏的稳定性存在影响,提示在制剂开发中,需关注辅料中氯乙酸对带负电荷或未共享电子对等易发生亲核反应原料药质量的影响。     

2,4-噻唑二酮的合成

氯乙酸和硫脲在乙醇中反应环合成2-亚氨基-4-噻唑酮盐酸盐，然后经酸性水解得到2，4-噻唑二酮，总收率为67.8%。     

Acylation of C-amino-s-triazoles with alpha-substituted carboxylic acid

Acylation of C-Amino-s-triazoles with α-Substituted Carboxylic Acid Derivatives The reaction of C-amino-s-triazoles ( 1 ) with lactic acid ( 2a ) or ethyl lactate ( 2b ) leads to the corresponding 3-lactoylamino-s-triazoles ( 3a, 3b ). Formation of the particular 3-[α-halo-acylamino]-s-triazoles ( 3c, 3e ) is the result of the action of α-halo-carboxylic acid esters or α-halocarboxylic acid halides ( 2c, 2d, 2e ) on 3-amino-s-triazole ( 1a ). Analogously, 3,5-bis[chloroacet-amino]-s-triazole ( 3d ) is formed from 3,5-diamino-s-triazole ( 1b ) and the chloroacetic acid derivatives 2c and 2d .     

Synthesis of heterocyclic quinones containing bridgehead nitrogen atom from 2-aminonaphtho[2,3-d]thiazole-4,9-dione

Imidazonaphthothiazole derivatives 3-6 were prepared by treatment of 2-aminonaphtho[2,3-d]-thiazole-4,9-dione(1) with phenacyl bromide, chloroacetic acid, diethyl oxalate and 2,3-dichloroquinoxaline respectively. The reaction of 1 with ethyl acrylate, ethyl acetoacetate and diethyl malonate gave the corresponding naphthothiazolopyrimidine derivatives 8-11.     

Synthesis of 1-,2-, and 3-(aminoacetyl)indoles and 1-(aminoacetyl)indolines (author's transl)

Synthesis of 1-, 2-, and 3-(Aminoacetyl)indoles and 1-(Aminoacetyl)indolines The chloroacetyl derivatives of various indoles and indolines, prepared by the reaction of the parent compounds with derivatives of chloroacetic acid derivatives, were reacted with amines to yield the title compounds.     

醋氯芬酸的合成

目的合成醋氯芬酸.方法以氯乙酸为原料,和2,3-二氢吡喃酯化反应合成氯乙酸四氢吡喃酯,再经缩合、酸解反应制得目标化合物.结果及结论本工艺操作简单,适合工业化生产,总产率达87%,制备出产品纯度较高.     

Synthesis and reactions of some new substituted pyridine and pyrimidine derivatives as analgesic, anticonvulsant and antiparkinsonian agents

A series of substituted pyridine and pyrimidine derivatives were synthesized as analgesic, anti convulsant, and antiparkinsonian agents by using compounds 1, 2, and 9 as starting materials. Pyr idino-imide derivative 3 was prepared by condensation of 1 with tetrachlorophthalic anhydride and compounds 4 and 5 were also obtained by reaction of compound 1 with 1,2,4,5-benzene-tetra carboxylic dianhydride and 1,4,5,8-naphthalenetetracarboxylic dianhydride, respectively. Similarly, compound 2 was reacted with previous anhydrides to afford the corresponding imide 6 and bis-imide derivatives 7 and 8, respectively. Bis-arylmethylene derivatives 9 were treated with hydrogen peroxide to afford the corresponding bis-oxiranocycloalkanone derivatives 10, which condensed with thiourea to give the corresponding thioxopyrimidine derivatives 11. Treatment of compound 11 with chloroacetic acid in the presence of anhydrous sodium acetate afforded the corresponding thiazolopyrim idine derivative 12 which condensed with aromatic aldehydes in acetic acid/acetic anhydride to give arylmethylene derivative 13. Also, compounds 13 could be prepared by reaction of compounds 11 with chloroacetic acid, aromatic aldehydes, and sodium acetate in a mixture of acetic acid and acetic anhydride. The pharmacological screening showed that many of these obtained compounds have good analgesic, anticonvulsant, and antiparkinsonian activities comparable to Valdecoxib, Carbamazepine, and Benzatropine as reference drugs.     

铋、铝、钙、镁混合盐类的乙二胺四乙酸二钠盐电流滴定法

在治疗胃病的药物中,有很多是铋、铝、钙、镁盐类的混合物,测定这些混合物中各成分的含量,如按照经典的方法,是非常耗时的。Brookes及Johnson两氏曾采用乙二胺四乙酸二纳盐(Na_2H_2Y,以下简称EDTA)作为滴定剂,在不同的pH值并应用多种指示剂,对该类药物中的各成分拟就比较简易的容量测定方法,然而它的应用范围仍受着许多的限制。后来,Reilly,Scribner及Temple三氏又利用EDTA在不同pH值与各种金     

肿瘤化学治疗的研究 ⅩⅦ.5-烷氧基和5-取代苯氧基嘧啶化合物的合成

本文报导了一系列5-烷氧基和5-取代苯氧基硫氧嘧啶(Ⅳ,Ⅴ)、5-烷氧基和5-取代苯氧基尿嘧啶(Ⅵ,Ⅶ)、5-烷氧基-和5-取代苯氧基-4-徑基-2-羧甲硫基嘧啶(Ⅷ,Ⅸ)及5-取代苯氧基-2-氨基-4-羟基嘧啶(Ⅹ)等化合物的合成,以进行抗肿瘤試驗. 初步药理試驗結果显示:化合物(Ⅳ₁),(Ⅳ₄),(Ⅴ₄),(Ⅴ₆),(Ⅴ₇),(Ⅵ₃),(Ⅶ₈),(Ⅶ₁₅),(Ⅶ₁₆),(Ⅸ₇)和(Ⅹ₁)对肉瘤180有明显的抑制作用.     

Reaktionen von 4,5-Diamino-s-triazolen mit Chloressigester und Oxalsäurediäthylester

Reactions of 4,5-Diamino-s-triazoles with Ethyl esters of Chloroacetic and Oxalic Acid By action of the ethyl ester of chloroacetic acid on 3-alkyl(alkyl)-4,5-diamino-s-triazoles I 3-alkyl(aryl)-4-amino-5-carbethoxymethylamino-s-triazoles, are formed of which some reactions are studied. The ethyl ester of oxalic acid with I formes N.N′-bis[3-alkyl-4-amino-s-triazolyl-(5)]-oxamides besides N-[3-alkyl-4-amino-s-triazolyl-(5)]-oxalesteramides. The former compound gives by hydrolysis s-triazolo-[4,3-b][1,2,4]triazine-6,7-dione and I.