N-1-苄基-3-甲基哌嗪置于5% Palladium Over Charcoal 氢气体系中,用 水 用作溶剂,化学反应 6.0H,以99%的收率获得2-甲基哌嗪 参考文献:Process For Producing Nitrogenous Heterocyclic Compound 标题:Process For Producing Nitrogenous Heterocyclic Compound 摘要:通过在水基溶剂中,在催化剂的存在下,用常压氢对n-取代的氮杂环化合物进行氢解,可以制备氮杂环化合物,如3-氨基吡咯啉衍生物.如果使用具有光学活性的1-取代-3-氨基吡咯啉衍生物作为原料,则可以在实际上不经过消旋作用的情况下获得光学活性的3-氨基吡咯啉衍生物作为产物.
专利信息
专利号:WO-9837078-A1 优先权日:1997-02-20 标题 :Solid phase and combinatorial synthesis of substituted thiophenes and of arrays of substituted thiophenes 发明人:DOERWALD FLORENCIO ZARAGOZA 权利人:NOVO NORDISK AS 摘要:A solid phase method for the synthesis of a plurality of differently substituted thiophenes with a wide variety of side-chain substituents as compounds of potential therapeutic interest. The thiophenes are prepared by reaction of a substrate-bound primary or secondary amine with a thiophosgene equivalent and reaction of the resulting intermediate with an acceptor-substituted acetonitrile in the presence of a base. Alkylation with an appropriate alkyl halide, followed by Thorpe-Ziegler-cyclization yields differently substituted, support-bound 3-aminothiophenes. These may be screened on the substrate or cleaved from the substrate and then screened in solution. Alternatively, the resin-bound 3-amino thiophenes or the synthetic intermediates can be subjected to further synthetic transformations (N-acylation, reduction) on the support, which permits the preparation of further therapeutically interesting compounds. The efficient synthesis of a wide variety of thiophenes using automated synthesis technology of the present method makes these compounds attractive candidates for the generation and rapid screening of diverse thiophene-based libraries. The method disclosed here provides an easy and fast access to highly diverse heterocyclic compounds of therapeutic interest, amenable to automatization.
专利号:WO-9740025-A1 优先权日:1996-04-19 标 题 :Solid phase and combinatorial synthesis of substituted 1,2,3-triazoles and of arrays of substituted 1,2,3-triazoles 发明人:DOERWALD FLORENCIO ZARAGOZA 权利人:NOVO NORDISK AS; DOERWALD FLORENCIO ZARAGOZA 摘要:A solid phase method for the synthesis of a plurality of differently substituted 1,2,3-triazoles with a wide variety of side-chain substituents as compounds of potential therapeutic interest. The 1,2,3-triazoles are prepared by acylation of a substrate-bound primary or secondary amine with a 3-oxoalkanoic acid and reaction of the resulting amide with a primary amine under dehydrating conditions to give an enamine. Treatment of this substrate-bound enamine with a sulfonyl azide in the presence of a base gives the corresponding 1,2,3-triazoles. These may be screened on the substrate or cleaved from the substrate and then screened in solution. The efficient synthesis of a wide variety of 1,2,3-triazoles using automated synthesis technology of the present method makes these compounds attractive candidates for the generation and rapid screening of diverse triazole-based libraries. The method disclosed here provides an easy and fast access to highly diverse heterocyclic compounds of therapeutic interest, amenable to automatization.
专利号:US-6136984-A 优先权日:1996-04-22 标 题 :Solid phase and combinatorial synthesis of substituted thiophenes and of arrays of substituted thiophenes 发明人:DOERWALD FLORENCIO ZARAGOZA 权利人:NOVO NORDISK AS 摘要:A solid phase method for the synthesis of a plurality of differently substituted thiophenes with a wide variety of side-chain substituents as compounds of potential therapeutic interest is disclosed. The thiophenes are prepared by acylation of a substrate-bound primary or secondary amine with cyanoacetic acid and reaction of the resulting cyanoacetamide with an isothiocyanate in the presence of a base. Alkylation with an appropriate alkyl halide, followed by Thorpe-Ziegier-cyclization yields differently substituted, support-bound 3-aminothiophenes. These may be screened on the substrate or cleaved from the substrate and then screened in solution. Alternatively, the resin-bound 3-amino thiophenes or the synthetic intermediates can be subjected to further synthetic transformations (N-acylation, reduction) on the support, which permits the preparation of further therapeutically interesting compounds. The efficient synthesis of a wide variety of thiophenes using automated synthesis technology of the present method makes these compounds attractive candidates for the generation and rapid screening of diverse thiophene-based libraries. The method disclosed here provides an easy and fast access to highly diverse heterocyclic compounds of therapeutic interest, amenable to automatization.
专利号:US-5847150-A 优先权日:1996-04-24 标题 :Solid phase and combinatorial synthesis of substituted 2-methylene-2, 3-dihydrothiazoles and of arrays of substituted 2-methylene-2, 3-dihydrothiazoles 发明人:DORWALD FLORENCIO ZARAGOZA 权利人:NOVO NORDISK AS 摘要:A solid phase method for the synthesis of a plurality of differently substituted 2-methylenethiazoles with a wide variety of side-chain substituents as compounds of potential therapeutic interest. The 2-methylenethiazoles are prepared by acylation of a substrate-bound primary or secondary amine with cyanoacetic acid and reaction of the resulting cyanoacetamide with an isothiocyanate in the presence of a base. Alkylation with an appropriate alkyl halide under acidic conditions yields differently substituted, support-bound 2-methylene-2,3-dihydrothiazoles. These may be screened on the substrate or cleaved from the substrate and then screened in solution. The efficient synthesis of a wide variety of 2-methylenethiazoles using automated synthesis technology of the present method makes these compounds attractive candidates for the generation and rapid screening of diverse thiazole-based libraries. The method disclosed here provides an easy and fast access to highly diverse heterocyclic compounds of therapeutic interest, amenable to automatization.
专利号:US-11059914-B2 优先权日:2016-12-21 标题:Method for the continuous synthesis of a diene elastomer with lithium amide initiator 发明人:DIRE CHARLOTTE; DESSENDIER MARIE-HÉLÈNE 权利人:MICHELIN & CIE 摘要:A process for the continuous synthesis of a diene elastomer is provided. The synthesis is conducted by means of n reactors r1 to rn, considered to be continuous stirred-tank reactors, which are equipped with an internal stirring system. The reactors are arranged in series, n varying from 2 to 15, preferably from 2 to 9. The reactor r1 is fed by an input solution comprising a solvent, one or more monomer(s), an anionic polymerization initiator chosen from lithium amides and a polar agent. The conversion by weight C1 in the first reactor is less than 70%, and the total conversion by weight Cn at the outlet of the reactor rn is greater than or equal to 70%.
专利号:US-4092316-A 优先权日:1975-02-03 标题:Synthesis of C-alkyl-triethylenediamines 发明人:NIEH EDWARD C Y 权利人:TEXACO DEVELOPMENT CORP 摘要:A liquid phase synthesis of C-alkyl-triethylenediamines involves heating to elevated temperatures of from about 200° C to 300° C a suitable N-(2-hydroxyalkyl) piperazine feedstock in the presence of a catalytic amount of a pentavalent acidic phosphorus compound and then recovering the C-alkyl-triethylenediamine product from the resulting reaction product mixture.
[参考文献]: Sin Ho Kweon, Et Al. Induction Of Human Leukemia Cell Differentiation Via Pkc/mapk Pathways By Arsantin, A Sesquiterpene Lactone From Artemisia Santolina. Arch Pharm Res. 2015 Nov;38(11):2020-8.
合成参考文献
参考文献:10.1107/s1600536811006945 摘要:Rong T. Bis[(2S,4S)-4-(2-hy-droxy-eth-yl)-2-methyl-piperazine-1,4-diium] di-μ-chlorido-bis-[trichloridocadmium(II)]. Acta Crystallogr Sect E Struct Rep Online. 2011 Apr 01;67(Pt 4):m396.