阿佐昔芬的合成

以4-溴苯乙酮为起始原料,经溴化、与3-甲氧基苯硫酚缩合、分子内环合得6-甲氧基-2-(4-溴苯基)苯并[b]噻吩(5);5经溴化、氧化反应后,与4-[2-(1-哌啶基)乙氧基]苯酚缩合制得关键中间体3-{4-[2-(1-哌啶基)乙氧基]苯氧基}-6-甲氧基-2-(4-溴苯基)苯并[b]噻吩亚砜(7);7再经还原、脱甲...     

Synthesis of thiazolotriazepinones

The synthesis of 4,5-dihydro-7-phenylthiazolo[2,3-c][1,2,4]triazepin-3(2H)-one ( 4 ) from 2-propenoic acid 2-(4-phenyl-2-thiazolyl)hydrazide ( 14 ), is reported. A synthesis of 4 which was reported earlier by Mahajan, Sondhi and Ralhan (9), from 3-chloropropanoic acid 2-(4-phenyl-2-thiazolyl)hydrazide ( 3 ), is erroneous. We were able to cyclize 3 to 1-(4-phenyl-2-thiazolyl)-3-pyrazolidinone ( 5 ). The cyclizations of 14 to 4 and 3 to 5 are consistent with the Baldwin Rules for Ring Closure.     

吡啶高三蝶烯的合成

2-溴-4-甲基吡啶（1）经氯代和碘代反应合成了2-溴-4-碘甲基吡啶（3）,3和蒽酮（4）反应生成10,10-二（2-溴-4-吡啶甲基）-9（10H）蒽酮（5）,5在3 MPa下与NaOCH3反应得到10,10-二（2-甲氧基-4-吡啶甲基）-9（10H）蒽酮（6）,6经硼氢化钠还原得到蒽醇（7）,7在对甲苯磺酸催化...     

氯雷他定的合成

以N-甲基-4-哌啶酮和8-氯-10,11-二氢-4-氮杂-5H-二苯并[a,d]-5-环庚酮为原料,经McMurry反应得到8-氯-6,11-二氢-11-(1-甲基-4-哌啶烯基)-5H-苯并[5,6]庚环[1,2-b]吡啶,收率为83.9%,最后与氯甲酸乙酯反应得到氯雷他定,总收率为35.7%。对McMurry反应过程中产生的副产物3、4进行了分离、表征。     

Dorsomorphin的合成

以2-氯甲基吡啶盐酸盐为原料,经氰基化、缩合和环合反应制得4-（4-吡啶基）-1H-吡唑-5-胺（5）; 5与2-（4-甲氧基苯基）丙二醛经缩合反应制得化合物6-（4-甲氧基苯基）-3-（4-吡啶基)吡唑并［1,5-a］嘧啶（9）; 9经脱甲基和成醚反应合成了骨形态生成蛋白受体及腺苷酸活化蛋白激酶抑制剂Dorsomorphin,总收率24%,其结构经¹H NMR和MS(ESI)确证。     

Synthesis of lonapalene

An efficient and practical synthesis of the antipsoriatic drug Lonapalene is reported. This involves the thermal rearrangement of 4-(4-chlorophenyl)-4-hydroxy-2,3- dimethoxycyclobutenone to 6-chloro-1,4-dihydroxy-2,3-dimethoxynaphthalene which was converted to Lonapalene upon treatment with acetic anhydride/pyridine.     

氮杂类聚合大环化合物的合成

以间苯二甲酰氯为原料, 分别与二(4-氨基苯基)甲烷、二(4-氨基苯基)醚及二(4-氨基苯基)砜通过一步反应合成了3种新的[3＋3]氮杂类聚合大环化合物, 产率分别为41%, 40%和36%; 并通过元素分析, IR, 1H NMR,13C NMR和MS对其结构进行了表征.     

Synthesis of 4-Aminosalicylglycine

To search for a better prodrug of 4-aminosalicylic acid that is expected to deliver stably parent drug to colon against the inflammatory bowel disease, a novel 4-aminosalicylic acid derivative was designed and synthesized from 4-aminosalicylic acid. 4-Aminosalicylglycine was prepared from 4-aminosalicylic acid by protecting amino and hydroxyl groups with benzyloxycarbonyl and acetyl, respectively, then the carboxylic acid was converted to acyl chloride which was treated with glycine. After removing the protection groups, 4-aminosalicylglycine wasobtained. All the compounds were characterized by FT-IR, ^1H-NMR, ^13C-NMR spectra. In vivo experiment on rats suggested that the curative effect of 4-aminosalicylglycine was more effective than that of 4-aminosalicylic acid.     

4-氰基吡啶的合成

以4-甲基吡啶为原料,在固定床反应器中通过含氧化钒的催化剂发生气固相接触氨氧化反应制备雷米封中间体4-氰基吡啶,4-甲基吡啶的转化率为99％,4-氰基吡啶的选择性为88％,收率为87．12％。     

Synthesis of nectriapyrone

A totally synthetic route to the antibacterial fungal metabolite nectriapyrone ( 1 ) has been achieved by condensation of methylmalonyl dichloride with ethyl trans-4-methyl-3-oxo-4-hexenoate followed by hydrolysis, decarboxylation, and methylation of the resulting 3-methyl-4-hydroxy-5-carbethoxy-6-(trans-1-methyl-1-propenyl)-2-pyrone. Exploration of an alternate scheme involving the dehydrogenation of 6-substituted-4-methoxy-5,6-dihydro-2-pyrones, prepared by Reformatsky reaction of ethyl γ-bromo-β-methoxycrotonate with various aldehydes, was abandoned since it did not appear to have general applicability to the preparation of nectriapyrone and its analogs.     

Synthesis of formyl-substituted porphyrins

Syntheses of 1, 4, 5, 8-tetramethyl-2-ethoxycarbonyl-6-formylporphyrin and 1, 4, 5, 8-tetramethyl-2, 3-diethoxycarbonyl-6-formylporphyrin from the copper complexes of 1, 4, 5, 8-tetramethyl-2-ethoxycarbonylporphyrin and 1, 4, 5, 8-tetramethyl-2, 3-diethoxycarbonylporphyrin are described.     

新型螺环树状化合物的合成

利用环己二酮单腙芳构化反应, 得到9H, 9H, 11H, 11H, 12H, 12H-六氢化苯并[9,10]-(1H, 1H, 3H, 3H, 4H, 4H, 5H, 5H, 7H, 7H, 8H, 8H-十二氢)菲-2, 6, 10-三酮腙, 然后与季戊四醇反应, 得到9H, 9H, 11H, 11H, 12H, 12H-六氢化苯并[9,10]-(1H, 1H, 3H, 3H, 4H, 4H, 5H,5H, 7H, 7H, 8H, 8H-十二氢)菲-2,6,10-三酮缩三(2,2-二羟甲基-1,3-丙二醇), 再与9-[4-(2,6-二硫杂环己基)苯基]-3-[4-(二甲酯基甲基)苯基]-2,4,8,10-四氧杂螺[5.5]十一烷反应, 制成标题化合物. 中间体和标题化合物经过IR, 1H NMR, MS和元素分析表征.     

4-正戊基环己酮的合成

以骨架镍催化4－正戊基苯酚加氢得到4－正戊基环己醇，再经氧化作用合成了4－正戊基环己酮，并探讨了催化加氢反应中的溶剂化作用。     

Synthesis of 4-aminocycloheptimidazoles

2-Methyl- 1a , 2-phenyl- 1b , and 2-amino-4-(2-methyl-1,3-dioxolan-2-yl)cycloheptimidazole ( 1c ) were treated with hydrazoic acid to give the corresponding 4-aminocycloheptimidazoles, respectively. However, the reaction of 4-(2-methyl-1,3-dioxolan-2-yl)cycloheptimidazole gave complex material. Some approaches to the synthesis of 4-aminonocycloheptimidazole itself are also described.     

Synthesis of Calix

The formation of p-tert-butylcalix[4]arene mono-, bis-, tris-, and tetrakistriflates 3, 2, 4, and 5, respectively, and their respective reactions, under typical Pd-catalyzed carbonylative, Suzuki-Miyaura coupling, or deoxygenation conditions are described. A novel, nonsolvent-derived 1:1 clathrate (6) of benzophenone and 3 was formed from the palladium-catalyzed carbonylative reaction of phenylboronic acid and 2. The X-ray crystal structure of this first nonsolvent-derived clathrate of a calix[4]arene derivative is reported. Another 1:1 clathrate of triethylamine and 3 was formed during the attempted Pd-catalyzed deoxygenation of 2.     

甲磺酸卡莫他特的合成

甲磺酸卡莫他特是口服有效的丝氨酸蛋白酶抑制剂。文献的合成方法有二种。其中一种为化合物3先与SOCl2反应成酰氯后,再与化合物2反应。     

单斜BiV04的离子液体辅助水热合成及表征

在离子液体[BMIM]Br辅助的水热条件下,合成了斜钒铋矿(Clinobisvanite,m-BiVO4)片状多面体微米晶.采用XRD,XPS,IR和SEM等对产物物相、结构和形貌进行了表征.结果表明,m-BiVO4产物为单斜晶系,I2/b空间群,片状多面体长宽为8～12 m,厚度为2-5 μm,晶型较完整,且具有良好...     

叶酸拮抗剂Alimta的合成

吡咯并[2,3-d]嘧啶类叶酸拮抗剂Alimta (1)是一种多靶向的抗癌药物, 本工作建立了新的方法全合成该药物. 通过Friedel-Crafts反应、黄鸣龙反应制备了4-(4-乙氧基-4-氧正丁基)苯甲酸乙酯(5), 收率为36.6%. 然后采用KBH₄/LiBr对5选择性还原, 再经氧化、成环等反应最终合成该药. 总收率4.8%.     

Synthesis of N-tetrahydropyranyl-S-methylmethioninesulfonium salts

D,L-Methionine reacts in alkaline medium with 4-methyl-3,4-epoxytetrahydropyran via the amino group to form, in accordance with the Krasusskii rule, an oxirane ring opening product, namely N-(4-hydroxy-4-methyl-3-tetrahydropyranyl)-D,L-methionine. N-(4-Hydroxy-4-methyl-3-tetrahydropyranyl)-S-methylmethioninesulfonium salts are synthesized in high yields by methylating the latter then treating it with organic or inorganic acids.Bashkir State University, Ufa. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 5, pp. 597–600, May, 1994. Original article submitted February 10, 1994.     

Synthesis of Isatin Derivatives

Reactions were studied of isatin sodium salt with bromocyclohexane, p-ethoxyphenyl chloroethyl ketone, 4,4'-di(chloromethyl)biphenyl, and 4,4'-(dichloromethyl)diphenylmethane. N-cyclohexylisatin, p-ethoxyphenyl N-isatinoethyl ketone, 4,4'-di(N-isatinomethyl)biphenyl, 4-chloromethyl-4'(N-isatinomethyl)biphenyl, 4,4'-di(N-isatinomethyl)diphenylmethane, 4-chloromethyl-4'(N-isatinomethyl)diphenylmethane, and 4-(N-morpholinomethyl)-4'-(N-isatinomethyl)diphenyl were synthesized.