2-羟基苯乙酮置于sodium Tetrahydroborate 盐酸,甲醇,Manganese(Iv) Oxide,Sodium Tetrahydroborate,4 A Molecular Sieve体系中,用 乙醚,二氯甲烷 作为反应溶剂,化学反应 20.0H,反应生成 2-苯基哌嗪 参考文献:Preparation Of Quinoxalines,Dihydropyrazines,Pyrazines And Piperazines Using Tandem Oxidation Processes 标题:Preparation Of Quinoxalines,Dihydropyrazines,Pyrazines And Piperazines Using Tandem Oxidation Processes 摘要:α-羟基酮在mno2介导的氧化下,随后与芳香或脂肪族1,2-二胺原位捕获,分别反应生成喹喔啉或二氢吡嗪,这一过程在一个反应釜中完成,避免了分离高度反应性1,2-二酮中间体的需要.对该工艺的修改可以反应生成吡嗪和吡咯啉. DOI:10.1039/b307177B
专利号:US-6603003-B2 优先权日:2000-11-07 标 题 :Method for the preparation of piperazine and its derivatives 发明人:SEBASTIAN SONNY; PATEL HETAL VIRENDRA; THENNATI RAJAMANNAR 权利人:SUN PHARMACEUTICAL IND LTD 摘要:A novel method for the synthesis of piperazine and its derivatives of formula 1,wherein R is selected from hydrogen, or a lower alkyl group having 1 to 6 carbon atoms or a phenylalkyl group the alkyl of which has 1 to 4 carbon atoms;R1 is selected from hydrogen, a methyl group, a phenyl group optionally substituted with an alkyl group having 1 to 6 carbon atoms, or a phenylalkyl group the alkyl of which has 1 to 4 carbon atoms; andR2 is selected from hydrogen, or a methyl group, or a fluoromethyl group;comprising the steps:a. reacting an ester of formula 11 with substituted or unsubstituted ethylenediamine of formula 7 to give 3,4-dehydropiperazine-2-one and its derivatives of formula 12, wherein R, R1, R2 are as defined above and R6 is a C1 to C4 linear or branched alkyl group; andb. reacting the 3,4-dehydro-piperazine-2-one and its derivatives of formula 12 with a reducing agent to yield the piperazine and its derivatives of formula 1.
专利号:WO-0062782-A1 优先权日:1999-04-19 标题 :Novel synthesis and crystallization of piperazine ring-containing compounds 发明人:SINGER CLAUDE; LIBERMAN ANITA; FINKELSTEIN NINA 权利人:TEVA PHARMA; TEVA PHARMA; SINGER CLAUDE; LIBERMAN ANITA; FINKELSTEIN NINA 摘要:The present invention is directed to methods for the preparation of piperazine ring-containing compounds, particularly mirtazapine. According to the present invention, the mirtazapine intermediate 1-(3-carboxypyridyl-2)-4-methyl-2-phenyl-piperazine is made by hydrolyzing 1-(3-cyanopyridyl-2)-4-methyl-2-phenyl-piperazine with a base where the base is present in a ratio of up to about 12 moles of the base per one mole of 1-(3-cyanopyridyl-2)-4-methyl-2-phenyl-piperazine. The mirtazapine intermediate 1-(3-carboxypyridly-2)-4-methyl-2-phenyl-piperazine may be made by hydrolyzing 1-(3-cyanopyridyl-2)-4-methyl-2-phenyl-piperazine with potassium hydroxide at a temperature of at least about 130 °C. The method of the present invention also includes reacting 2-amino-3-hydroxymethyl pyridine with N-methyl-1-phenyl-2, 2'-iminodiethyl chloride to form 1-(3-hydroxymethylpyridyl-2)-4-methyl-2-phenyl piperazine, and adding sulfuric acid to the 1-(3-hydroxymethylpyridyl-2)-phenyl-4-methylpiperazine to form mirtazapine. The present invention also relates to new processes for recrystallization of mirtazapine form crude mirtazapine.
专利号:WO-2006079916-A1 优先权日:2005-01-26 标 题 :Thieno [2,3-d] pyrimidine compounds as inhibitors of adp-mediated platelets aggregation 发明人:ENNIS MICHAEL DALTON; KORTUM STEVEN WADE; RAHMAN HAYAT; SCHWEITZER BARBARA ANN; TENBRINK RUTH ELIZABETH 权利人:PHARMACIA & UPJOHN CO LLC; ENNIS MICHAEL DALTON; KORTUM STEVEN WADE; RAHMAN HAYAT; SCHWEITZER BARBARA ANN; TENBRINK RUTH ELIZABETH 摘要:Compounds and pharmaceutically acceptable salts of the compounds are disclosed, wherein the compounds have the structure of Formula (I): wherein A1, A2, A3, A4, A5, A6, A7, A8, X4, X6, R2, R4, R5, and R6 are as defined in the detailed description of the invention. Corresponding pharmaceutical compositions, methods of treatment, methods of synthesis, and intermediates are also disclosed.
专利号:WO-2007144409-A1 优先权日:2006-06-16 标 题:Stereoselective synthesis of (s)-1-methyl-3-phenylpiperazine
专利号:US-6936600-B2 优先权日:1999-04-01 标题:Sorbitol dehrydrogenase inhibitors 发明人:CHU-MOYER MARGARET Y; MYLARI BANAVARA L; ZEMBROWSKI WILLIAM J 权利人:PFIZER 摘要:This invention is directed to sorbitol dehydrogenase inhibitory compounds of the formula I, n n nwherein R 1 , R 2 and R 3 are as defined in the specification. This invention is also directed to pharmaceutical compositions containing those compounds and methods of treating or preventing diabetic complications, particularly diabetic neuropathy, diabetic nephropathy, diabetic microangiopathy, diabetic macroangiopathy and diabetic cardiomyopathy by administering such compounds to a mammal suffering from diabetes and therefore at risk for developing such complications. This invention is also directed to pharmaceutical compositions comprising a combination of a compound of formula I of this invention with an aldose reductase inhibitor and to methods of treating or preventing diabetic complications therewith. This invention is also directed to pharmaceutical compositions comprising a combination of a compound of formula I of this invention with an NHE-1 inhibitor and to methods of treating cardiomyopathy and other heart-related problems therewith. This invention is also directed to certain intermediates used in the synthesis of the compounds of formula I and to processes for preparing those intermediates.
专利号:US-6734307-B2 优先权日:2000-07-17 标 题:Oxazolidinone derivatives as antimicrobials 发明人:MEHTA ANITA; SUDERSHAN ARORA K; DAS BISWAJIT; RAY ABHIJIT; RUDRA SONALI; RATTAN ASHOK 权利人:RANBAXY LAB LTD 摘要:The present invention relates to certain substituted phenyl oxazolidinones and to processes for the synthesis of the same. This invention also relates to pharmaceutical compositions containing the compounds of the present invention as antimicrobials. The compounds are useful antimicrobial agents, effective against a number of human and veterinary pathogens, including gram-positive aerobic bacteria such as multiply-resistant staphylococci, streptococci and enterococci as well as anaerobic organisms such as Bacterioides spp. and Clostridia spp. species, and acid fast organisms such as Mycobacterium tuberculosis, Mycobacterium avium and Mycobacterium spp.
参考文献:10.3797/scipharm.1012-17 摘要:Bielenica A, Kossakowski J, Struga M, Dybała I, Loddo R, Ibba C, La Colla P. Synthesis and Biological Evaluation of New 3-Phenyl-1-[(4-arylpiperazin-1-yl)alkyl]-piperidine-2,6-diones. Sci Pharm. 2011 Apr;79(2):225–38.