2-氨基烟酸置于diethylphosphoryl Cyanide,氯化铵,三乙胺体系中,用 乙二醇二甲醚,苯 用作溶剂,化学反应 2.0H,反应生成2-氨基-3-氰基吡啶 参考文献:Pyrido[2,3-D]Pyrimidine Derivatives: Synthesis Via The Intermolecular Aza-Wittig Reaction/heterocyclization And The Crystal Structure 标题:Pyrido[2,3-D]Pyrimidine Derivatives: Synthesis Via The Intermolecular Aza-Wittig Reaction/heterocyclization And The Crystal Structure 摘要: Doi:10.1055/s-1998-2170
专利号:WO-2009127773-A1 优先权日:2008-04-15 标 题:Method of using an electric field in the synthesis of materials 发明人:REIJONEN MIKA TAPIO 权利人:REIJONEN MIKA TAPIO 摘要:A synthesis method using polarization of materials by an electric field consists of two electrodes (1 and 4), an insulation layer (2), a dielectric layer (3) where the synthesis takes place, a voltage supply (5), a closed circuit and a synthesis container.
专利号:US-3950160-A 优先权日:1972-09-27 标题:Inhibiting the growth of weeds with 2-substituted pyrdidopyimidines and salts thereof 发明人:ABU EL-HAJ MARWAN J; DOMINY BERYL WILLIAM 权利人:PFIZER 摘要:2-Substituted pyridopyrimidines and their alkali and alkylamine salts as herbicides, and processes for the synthesis of starting materials leading to the preparation thereof.
专利号:US-2003069417-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 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-carboxypyridyl-2)-4-methyl-2-phenyl-piperazine may be made of 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 a recrystallization of mirtazapine from crude mirtazapine. The present invention also relates to crystalline adducts of mirtazapine and water, preferably containing up to about 3.5% by weight water, pharmaceutical compositions containing the crystalline adducts, and methods of treating depression by administering such compositions.
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:US-6576764-B2 优先权日:1999-04-19 标 题:Synthesis and crystallization of piperazine ring-containing compounds 发明人:SINGER CLAUDE; LIBERMAN ANITA; FINKELSTEIN NINA 权利人:TEVA PHARMA 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-carboxypyridyl-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 from crude mirtazapine.
专利号:US-3962264-A 优先权日:1972-09-27 标 题:Process for making 2-amino nicotinonitrile 发明人:ABU EL-HAJ MARWAN J; DOMINY BERYL WILLIAM 权利人:PFIZER 摘要:2-Substituted pyridopyrimidines and their alkali and alkylamine salts as herbicides, and processes for the synthesis of starting materials leading to the preparation thereof.
摘要:Walker, J. C. L., Science of Synthesis: Knowledge Updates, (2024) 3, 222. 参考文献:10.1107/s1600536810027479 摘要:Shi D, Yang L, Tang J, Wang X, Li J. Spiro[cyclopentane-1,2′(1′H)-pyrido[2,3-d]pyrimidin]-4′(3′H)-one. Acta Crystallogr E Struct Rep Online. 2010 Aug 18;66(9):o2301. doi: 10.1107/s1600536810027479.