4-溴-2-硝基苯甲酸置于0.82Mol% Pd/c,氢气,碳酸氢钠体系中,用 甲醇 作为反应溶剂,化学反应 0.42H,以92%的收率获得产物邻硝基苯甲酸 参考文献:Reductive Dehalogenation Of Aryl Bromides And Chlorides And Their Use As Aryl Blocking Groups 标题:Reductive Dehalogenation Of Aryl Bromides And Chlorides And Their Use As Aryl Blocking Groups 摘要:溴取代基和氯取代基是芳香环上极好的封端基团.当卤代基对位正,副定向基团时,正交位置很容易被官能化,卤代基随后可在中性条件下通过催化氢化作用去除.不出所料,溴化物的还原速度比氯化物快,反应所需的催化剂也较少.在存在硝基,氯基,氰基,酮基或羧酸基团的情况下,可选择性地还原溴化物. DOI:10.1055/s-0029-1217112
专利号:US-2021107859-A1 优先权日:2018-04-06 标题 :A process for the synthesis of carbon labeled organic compounds 发明人:AUDISIO DAVIDE; CANTAT THIBAULT; DESTRO GIANLUCA 权利人:COMMISSARIAT ENERGIE ATOMIQUE 摘要:A process for the synthesis of a carbon labeled organic compound containing a carbon labeled carboxyl group is described. A method of using carbon labeled organic compounds containing a carbon labeled carboxyl group according to the present disclosure; a process for manufacturing labeled pharmaceuticals and agrochemicals comprising synthesis of carbon labeled organic compounds containing a carbon labeled carboxyl group according to the present disclosure; and a process for producing tracers comprising synthesis of carbon labeled organic compounds containing a carbon labeled carboxyl group according to the present disclosure are also described.
专利号:US-11613514-B2 优先权日:2016-03-25 标题:Crystal forms and methods of synthesis of (2R, 6R)-hydroxynorketamine and (2S, 6S)-hydroxynorketamine 发明人:THOMAS CRAIG; ZARATE CARLOS; MOADDEL RUIN; GOULD TODD; ZANOS PANOS; MORRIS PATRICK 权利人:US HEALTH; UNIV MARYLAND 摘要:The disclosure provides a method for synthesizing free base forms of (2R,6R)-hydroxynorketamine (HNK) and (2S,6S)-hydroxynorketamine. In an embodiment synthesis of (2R,6R)-hydroxynorketamine (HNK) includes preparation of (R)-norketamine via chiral resolution from racemic norketamine via a chiral resolution with L-pyroglutamic acid. The disclosure also provided crystal forms of the corresponding (2R,6R)-hydroxynorketamine (HNK) and (2S,6S)-hydroxynorketamine hydrochloride salts.
专利号:US-8722886-B1 优先权日:2012-11-13 标题:Methods for the total chemical synthesis of enantiomerically-pure 7-(2′-trimethylsilyl)ethyl camptothecin 发明人:CHEN XINGHAI; HAUSHEER FREDERICK H; MALAKHOV ANDREY; KOCHAT HARRY 权利人:CHEN XINGHAI; HAUSHEER FREDERICK H; MALAKHOV ANDREY; KOCHAT HARRY; BIONUMERIK PHARMACEUTICALS INC 摘要:The present invention discloses and claims five (5) novel, highly efficient synthetic routes for the total synthesis of enantiomerically-pure (i.e., 99%) 7-(2′-trimethylsilyl)ethyl camptothecin (BNP1350; Karenitecin; Cositecan). These aforementioned synthetic schemes are the first to disclose the total syntheses of 7-(2′-trimethylsilyl)ethyl camptothecin using a highly novel direct, non-linear and convergent synthetic strategy which involves annealing the key C7-(trimethylsilyl)ethyl side chain-bearing A ring key synthons to an enantiomerically-pure tricyclic pyridone; rather than through the conventional methodology which incorporates the C7-(trimethylsilyl)ethyl side chain as the final synthetic step on a totally synthesized camptothecin parent compound. The current novel synthetic approaches reported herein since utilize desirably functionalized A-ring with preinstalled trimethyl silyl ethyl side chain, the aforementioned synthetic methodologies have a wider scope of making wide range of pharmaceutically relevant A-ring substituted BNP1350 analogs by substituting desirably functionalized nitro or protected amino phenyl carboxy A-ring as the starting material.
专利号:US-7429658-B2 优先权日:2003-09-11 标题 :Synthesis of protected pyrrolobenzodiazepines 发明人:HOWARD PHILIP; MASTERSON LUKE 权利人:SPIROGEN LTD 摘要:A method of synthesis of a N-10 protected PBD compound of formula (I): n nvia an intermediate of formula (II) or formula (V):
专利号:US-10683318-B2 优先权日:2014-10-17 标 题:Scalable synthesis of reduced toxicity derivative of amphotericin B 发明人:BURKE MARTIN D; UNO BRICE E; RAKSHIT SOUVIK 权利人:UNIV ILLINOIS 摘要:Disclosed is a simplified, readily scalable series of individual methods that collectively constitute a method for the synthesis of C2′epiAmB, an efficacious and reduced-toxicity derivative of amphotericin B (AmB), beginning from AmB. Also provided are various compounds corresponding to intermediates in accordance with the series of methods.
专利号:US-7557099-B2 优先权日:2004-03-01 标题 :Pyrrolobenzodiazepines as key intermediates in the synthesis of dimeric cytotoxic pyrrolobenzodiazepines 发明人:HOWARD PHILIP WILSON; KANG GYOUNG-DONG 权利人:SPIROGEN LTD 摘要:Compounds and a method of synthesis of compounds of formula (Ia) or (Ib): and salts, solvates, and chemically protected forms thereof, wherein the dotted lines indicate the optional presence of a double bond between C1 and C2 or C2 and C3; R 2 and R 3 are independently selected from —H, â•?O, â•?CH 2 , —CN, —R, OR, halo, â•?CH—R, O—SO 2 —R, CO 2 R and COR; R 10 is a carbamate-based nitrogen protecting group; and R 11 is an oxygen protecting group.
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合成参考文献
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