4-甲基乙酰苯胺置于氯,铁粉,水,Sodium Hydroxide体系中,用 1,2-二氯乙烷 作为反应溶剂,以47 %的收率获得产物2-氯-4-甲基苯胺 参考文献: A Process For The Preparation Of 2-Chloro-4-Methylaniline[fr] Procédé De Préparation De 2-Chloro-4-Méthylaniline 标题: A Process For The Preparation Of 2-Chloro-4-Methylaniline[fr] Procédé De Préparation De 2-Chloro-4-Méthylaniline 摘要:The Present Invention Discloses A Novel,Efficient And Industrially Advantageous Process For The Preparation Of 2-Chloro-4-Methylaniline Of Formula I Comprising Chlorination Of N Protected Toluidine Of Formula Iii To Obtain N Protected Ortho Chloro Toluidine Of Formula Ii Which Is Further Deprotected To Obtain 2-Chloro-4-Methylaniline Of Formula I.
专利号:US-10005720-B2 优先权日:2013-04-05 标题:Compounds useful for the treatment of metabolic disorders and synthesis of the same 发明人:SEXTON JONATHAN Z; BRENMAN JAY E; MUSSO DAVID L 权利人:NORTH CAROLINA CENTRAL UNIV; UNIV NORTH CAROLINA CHAPEL HILL 摘要:The present invention provides compounds of Formula (I): wherein variables X, Y, Z and R1 are as described herein. Some of the compounds described herein are glutamate dehydrogenase activators. The invention is also directed to pharmaceutical compositions comprising these compounds, uses of these compounds and compositions in the treatment of metabolic disorders as well as synthesis of the compounds.
专利号:US-8653282-B2 优先权日:2007-10-18 标 题:Preparation of dihydrothieno [3,2-D] pyrimidines and intermediates used therein 发明人:FRUTOS ROGELIO; KRISHNAMURTHY DHILEEPKUMAR; MULDER JASON ALAN; RODRIGUEZ SONIA; SENANAYAKE CHRIS HUGH; TAMPONE THOMAS G 权利人:FRUTOS ROGELIO; KRISHNAMURTHY DHILEEPKUMAR; MULDER JASON ALAN; RODRIGUEZ SONIA; SENANAYAKE CHRIS HUGH; TAMPONE THOMAS G; BOEHRINGER INGELHEIM INT 摘要:The invention relates to improved methods of preparing dihydrothienopyrimidines of formula 1, and intermediates thereof, (I) wherein X is SO or SO 2 , preferably SO, and wherein R A , R 1 , R 2 , R 3 , R 4 and R 5 have the meanings given in the description. The methods according to this invention are more suitable for large-scale synthesis of said compounds than prior methods because the new synthetic process avoids distillation and chromatographic purification between steps and results in a higher overall yield of the desired product.
专利号:US-2018370905-A1 优先权日:2013-04-05 标题:Compounds Useful for the Treatment of Metabolic Disorders and Synthesis of the Same
专利号:US-5998595-A 优先权日:1996-11-05 标题:Azidohalogenobenzyl derivatives, sugar compounds and protection of hydroxy groups 发明人:KUSUMOTO SHOICHI; FUKASE KOICHI 权利人:WAKO PURE CHEM IND LTD 摘要:Azidohalogenobenzyl derivatives of the formula (I) ##STR1## wherein A is a halogen atom, B is a halogen atom or a hydrogen atom, and X is a group reactive with a hydroxy group, methods of protecting hydroxy group(s) using said derivatives, and sugar compounds wherein a hydrogen atom of at least one hydroxy group is substituted by an azidohalogenobenzyl group. According to the present invention, there are provided novel derivatives capable of introducing a group into a compound having hydroxy group(s), which group is useful as a stable hydroxy-protecting group even in solid phase synthesis for the purpose of the extension of sugar chain under continuous acidic conditions and of being removed under mild conditions; sugar compounds protected by using said derivatives; and methods of protecting hydroxy group(s) using said derivatives.
专利号:US-4136033-A 优先权日:1969-11-07 标 题:6-hydroxypyridone-2 compounds having a cationic group in the 3-position 发明人:STEINEMANN WILLY 权利人:SANDOZ LTD 摘要:Compounds of the formula ##STR1## wherein K.sup.⊕ is a cationic group, preferably heterocyclic, n R is hydrogen or an organic radical, preferably alkyl, phenyl or acyl, n R 1 is hydrogen, hydrocarbyl, substituted hydrocarbyl, heterocyclyl, substituted heterocyclyl, amino or substituted amino, and n A.sup.⊖ is an anion, n Are useful as intermediates in the synthesis of azo dyes of the formula ##STR2## wherein D is an aromatic carbocyclic or heterocyclic diazo component radical, and n K.sup.⊕, r, r 1 and A.sup.⊖ are as defined above.
专利号:US-2016046560-A1 优先权日:2013-04-05 标题 :Compounds useful for the treatment of metabolic disorders and synthesis of the same
[参考文献]: Miguel Del Nogal Sánchez, Et Al. A Method Based On Microextraction By Packed Sorbent-Programmed Temperature Vaporizer-Fast Gas Chromatography-Mass Spectrometry For The Determination Of Aromatic Amines In Environmental Water Samples. Anal Bioanal Chem. 2012 Oct;404(6-7):2007-15.
合成参考文献
摘要:Joule, J. A., Science of Synthesis Knowledge Updates, (2010) 2, 56. 摘要:Maison, W., Science of Synthesis Knowledge Updates, (2020) 1, 419. 摘要:Hay, M. B.; Hicks, J. D., Science of Synthesis: Cross Coupling and Heck-Type Reactions, (2012) 2, 114. 摘要:Hamilton, A., and H. L. Hardy. Industrial Toxicology. 3rd ed. Acton, Mass.: Publishing Sciences Group, Inc., 1974., p. 311 摘要:Schafer, E. W., Jr., W. A. Bowles Jr., and J. Hurlbut. 1983. The acute oral toxicity and repellency and hazard potential of 998 chemicals to one or more species of wild and domestic birds. Archives of Environmental Contamination and Toxicology 12:355-382. https://www.aphis.usda.gov/ws/nwrc/chem-effects-db/Q_schafer832.pdf