该化合物是有机合成中通常用作坚固基础和核素的有机石化合物,通常是作为液态碳氢化合物的一种溶液,如六氟或环乙烷,其浓度在1.0 M至2.5 M. n-Hexylithium之间,特别是在脱核和金属-卤素交换反应方面,高度反应性,使其对产生碳离子和启动电离聚合物具有价值.其线性乙基乙酰链与短链烷基共试剂相比,具有更高的溶性与稳定性.处理需要严格的惰性条件(例如氮/烷大气),因为其交火性性质和对水和氧的敏感性.在低温下适当储存对于保持再活性和储存寿命至关重要.
1-氯己烷置于sodium,Lithium体系中,用 正己烷 用作溶剂,20.0~40.0 °C,29.0 Kpa 条件下,反应 4.33H,以48.8%的收率获得正己基锂 参考文献:[de] Verfahren Zur Herstellung Von Alkyllithiumverbindungen Und Aryllithiumverbindungen Durch Reaktionsverfolgung Mittels Ir-Spektroskopie Method For Producing Alkyl Lithium Compounds And Aryl Lithium Compounds By Monitoring The Reaction By Means Of Ir-Spectroscopy[fr] Procede De Production De Compose Alkyle Lithium Et De Compose Aryle Lithium Avec Suivi De La Reaction Par Spectroscopie Infrarouge 标题:[de] Verfahren Zur Herstellung Von Alkyllithiumverbindungen Und Aryllithiumverbindungen Durch Reaktionsverfolgung Mittels Ir-Spektroskopie Method For Producing Alkyl Lithium Compounds And Aryl Lithium Compounds By Monitoring The Reaction By Means Of Ir-Spectroscopy[fr] Procede De Production De Compose Alkyle Lithium Et De Compose Aryle Lithium Avec Suivi De La Reaction Par Spectroscopie Infrarouge 摘要:描述了一种通过在溶剂中将锂金属与烷基或芳基卤化物反应制备烷基和芳基锂化合物的方法,其中通过在线测量在反应釜中的烷基/芳基卤化物和烷基/芳基锂化合物的浓度,利用红外光谱法进行评估,通过评估红外光谱测量,实现对卤化物组分的精确终点识别的剂量.这样可以实现最佳的反应控制和产率.通过对底物和产物各自浓度的了解,可以确保安全的反应控制.通过卤化物剂量的终点确定,可以优化反应产率,同时通过在反应过程中降低产品浓度来提高产品纯度.
专利号:WO-2019170521-A1 优先权日:2018-03-07 标题 :Synthesis of obeticholic acid and synthesis intermediate 发明人:BERNABEU MARTÃ?NEZ MARÃ?A DEL CARMEN; JIMÉNEZ ALONSO OSCAR; DOBARRO RODRÃ?GUEZ ALICIA; GABOARDI MAURO; CASTALDI GRAZIANO 权利人:MOEHS IBERICA SL 摘要:The present invention relates to a new intermediate for the synthesis of obeticholic acid, the compound of formula (I) or a geometric isomer thereof, a process for obtaining the same, as well as the use of said intermediate in the synthesis of obeticholic acid.
专利号:US-8273790-B2 优先权日:2005-01-14 标 题:Exo-selective synthesis of himbacine analogs 发明人:THIRUVENGADAM TIRUVETTIPURAM K; SUDHAKAR ANANTHA; LIM NGIAP KIE; KWOK DAW-IONG; WU GEORGE G; WANG TAO; HUANG MINGSHENG; GREEN MICHAEL D 权利人:THIRUVENGADAM TIRUVETTIPURAM K; SUDHAKAR ANANTHA; LIM NGIAP KIE; KWOK DAW-IONG; WU GEORGE G; WANG TAO; HUANG MINGSHENG; GREEN MICHAEL D; SCHERING CORP 摘要:This application discloses a novel process for the synthesis of himbacine analogs, as well as the compounds produced thereby. The synthesis proceeds by alternative routes including the cyclic ketal amide route, the chiral carbamate amide route, and the chiral carbamate ester route. The compounds produced thereby are useful as thrombin receptor antagonists. The chemistry disclosed herein is exemplified in the following synthesis sequence:
专利号:US-12162849-B2 优先权日:2018-12-21 标题 :Synthesis of 3-methyl-1,2,4-thiadiazole-5-carbohydrazide or of the methyl-d3 deuterated form thereof 发明人:HOVEYDA HAMID; DUTHEUIL GUILLAUME 权利人:OGEDA SA 摘要:The present invention relates to a method of synthesis of compound (I), wherein R1 represents methyl or methyl-d3, thus corresponding to 3-methyl-1,2,4-thiadiazole-5-carbohydrazide or to the methyl-d3 deuterated form thereof. These compounds are useful as key intermediates in the synthesis of pharmaceutical compounds, especially fezolinetant and deuterated fezolinetant.
专利号:US-2008103312-A1 优先权日:2006-08-29 标 题:Processes for the synthesis of 5-phenyl-1-trityl-1H-tetrazole 发明人:KANSAL VINOD K; MISTRY DHIRENKUMAR N; VASOYA SANJAY L; LUNAGARIYA VIJAYKUMAR D 权利人:KANSAL VINOD K; MISTRY DHIRENKUMAR N; VASOYA SANJAY L; LUNAGARIYA VIJAYKUMAR D 摘要:Provided are processes for the synthesis of 5-phenyl-1-trityl-1H-tetrazole, an intermediate useful in the synthesis of irbesartan.
专利号:US-2001044540-A1 优先权日:2000-03-23 标 题:Asymmetric synthesis of quinazolin-2-ones useful as HIV reverse transcriptase inhibitors 发明人:PARSONS RODNEY L; DOROW ROBERTA L; DAVULCU AKIN H; FORTUNAK JOSEPH M; HARRIS GREGORY D; KAUFFMAN GOSS S; NUGENT WILLIAM A; RADESCA LILIAN A 摘要:This invention relates generally to the asymmetric synthesis of quinazolin-2-ones that are useful as inhibitors of HIV reverse transcriptase. The synthesis is accomplished through the chiral ligand mediated addition of cyclopropylacetylide.
专利号:WO-2017063617-A1 优先权日:2015-10-13 标 题 :Preparation of intermediates for the synthesis of canagliflozin and dapagliflozin 发明人:ZEZULA JOSEF; BABIAK PETR; HAJDUCH JAN 权利人:ZENTIVA KS 摘要:The present invention relates to a preparation method of the intermediates of structures la (for the synthesis of canagliflozin) and 1b (for the synthesis of dapagliflozin), where in structure la X is methyl and Ar represents 2-(5-(4-fluorophenyl)-thienyl) and in structure 1b X is chlorine and Ar represents 4-ethoxyphenyl.
摘要:Kantchev, E. A. B.; Organ, M. G., Science of Synthesis, (2009) 48, 77. 摘要:Lete, E.; Sotomayor, N., Science of Synthesis Knowledge Updates, (2011) 4, 240. 摘要:Davies, G. H. M.; Wisniewski, S. R., Science of Synthesis Knowledge Updates, (2021) 2, 143. 摘要:Marek, I.; Basheer, A., Science of Synthesis: Stereoselective Synthesis, (2011) 1, 347. 摘要:Roy, M.-N.; Lindsay, V. N. G.; Charette, A. B., Science of Synthesis: Stereoselective Synthesis, (2011) 1, 804.