碘苯置于异丙基氯化镁体系中,用 四氢呋喃 用作溶剂,化学反应 0.92H,反应生成苯基氯化镁 参考文献:Process Safety Evaluation Of A Magnesium−iodine Exchange Reaction 标题:Process Safety Evaluation Of A Magnesium−iodine Exchange Reaction 摘要:An Unexpected Highly Exothermic Decomposition Was Observed During Routine Safety Analysis Of The Magnesium-Iodine Exchange Reaction Of 2-Iodo-4-Fluorotoluene ( 3) With Commercially Available I-Prmgcl (2.0 M Solution In Thf). When The Reaction Mixture Was Scanned In An Adiabatic Calorimeter With The Use Of A 2 Degrees C/min Temperature Ramp,A Rapid Exothermic Decomposition With An Onset Temperature Of Approximately 80 Degrees C Was Observed. The System Temperature Rapidly Rose To 210 Degrees C At A Peak Rate Of 200 Degrees C/min. Subsequent Testing Of Three Simplified Substrates Showed The Same Type Of Exothermic Decomposition For All Cases. Control Experiments Indicated That The Decomposition Requires Both Aryl Iodide And I-Prmgcl ( Or Arylmgcl And I-Pri). While The Onset Temperatures For All Cases Studied Were Generally Well Above The Typical Operating Temperature For These Reactions (0-10 Degrees C),It Is Nonetheless Important To Cautiously Evaluate These Types Of Processes And Install Proper Engineering Controls For Analogous Decomposition Events. Doi:10.1021/op060145B
专利信息
专利号:US-2006293466-A1 优先权日:2003-06-20 标 题:Methods for synthesis of graft polymers 发明人:GAUTHIER MARIO; YUAN ZHONGSHUN 权利人:UNIV WATERLOO 摘要:A process for the synthesis of arborescent polymers comprises epoxidation of a first polymer and grafting thereto a second polymer having groups reactive to the epoxide groups on the first polymer. The epoxidation and grafting steps can be repeated. In an additional embodiment, the present invention provides a one-pot method for the synthesis of arborescent polymers. In a reaction pot, a first polymer is copolymerized and then reacted with an activating compound in order to generate a polyfunctional macroinitiator. Monomers are then added to the reaction pot, the monomers having functional groups reactive towards reactive sites on the first polymer.
专利号:US-7148356-B2 优先权日:2001-07-13 标题:Process for the catalytic synthesis of biaryls and polymers from aryl compounds 发明人:SMITH III MILTON R; MALECZKA ROBERT E 权利人:UNIV MICHIGAN STATE 摘要:A process for producing organic substituted aromatic or heteroaromatic compounds including biaryl and biheteroaryl compounds in a two-step reaction. In the first step, the aromatic or heteroaromatic compound is borylated in a reaction comprising a borane or diborane reagent (any boron reagent where the boron reagent contains a B—H, B—B or B—Si bond) and an iridium or rhodium catalytic complex. In the second step, a metal catalyst catalyzes the formation of the organic substituted aromatic or heteroaromatic compound from the borylated compound and an electrophile such as an aryl or organic halide, triflate (OSO 2 CF 3 ), or nonaflate (OSO 2 C 4 F 9 ). The steps in the process can be performed in a single reaction vessel or in separate reaction vessels. The present invention also provides a process for synthesis of complex polyphenylenes starting from halogenated aromatic compounds.
专利号:US-5703223-A 优先权日:1994-09-02 标题 :Solid phase synthesis of oligonucleotides with stereospecific substituted phosphonate linkages by pentavalent grignard coupling 发明人:WICKSTROM ERIC; LE BEC CHRISTINE 权利人:UNIV JEFFERSON 摘要:The present invention provides a method for producing an oligonucleotide having stereospecific substituted phosphonate linkages by use of a pentavalent Grignard coupling reaction on a solid phase support. The method can be used for automated synthesis of oligonucleotides having sequential equatorial or axial stereospecific substituted phosphonate linkages.
专利号:US-4365094-A 优先权日:1979-12-28 标 题 :Process for the synthesis of tertiary phosphine oxides, and new tertiary phosphine oxides 发明人:BOILEAU SYLVIE L; N GUYEN THANH-DUNG; GAUTIER JEAN-CLAUDE C 权利人:POUDRES & EXPLOSIFS STE NALE 摘要:The invention relates to the synthesis of tertiary phosphine oxides and also to certain tertiary phosphine oxides. According to the invention, an organic phase containing a halogenomethyl derivative, a secondary phosphine oxide and a phase transfer catalyst in an organic medium is reacted with an aqueous phase containing an inorganic base. The halogenomethyl derivative can be a micromolecule or a macromolecule. The tertiary phosphine oxides are substances which are useful, in particular, in fireproofing, in hydrometallurgy and in the field of plant health.
专利号:US-5880295-A 优先权日:1994-02-16 标 题 :Process for the preparation of diamine intermediates useful in the synthesis of HIV protease inhibitors 发明人:KALTENBACH III ROBERT FRANK 权利人:DU PONT PHARM CO 摘要:The present invention provides a process for the preparation of compounds of formula (V) below, and analogs thereof, which are useful as intermediates for the synthesis of HIV protease inhibitors, including cyclic ureas. ##STR1##
专利号:WO-2015130660-A1 优先权日:2014-02-25 标题 :Synthesis of racemic amphetamine derivatives by cuprate addition reaction with aziridine phosphoramidate compounds 发明人:MECKLER HAROLD; GREGG BRIAN THOMAS; YANG JIE 权利人:Chemapotheca LLC 摘要:The invention includes processes for the synthesis of amphetamine, dexamphetamine, methamphetamine, derivatives of these, including their salts, and novel precursors and intermediates obtained thereby, by synthesizing aziridine phosphoramidate compounds in specified solvents at specified temperatures, and then converting to a novel aryl or aryl-alkyl phosphoramidate precursors using an organometallic compound such as a copper salt, where the novel aryl or aryl-alkyl phosphoramidate precursor is then easily converted to the target compounds using known reactions.
摘要:Black, D. A.; Fagnou, K., Science of Synthesis, (2010) 45, 602. 摘要:Ohno, H.; Tomioka, K., Science of Synthesis, (2008) 44, 94. 摘要:Black, D. A.; Fagnou, K., Science of Synthesis, (2010) 45, 636. 摘要:Gandon, V.; Malacria, M., Science of Synthesis, (2008) 44, 219. 摘要:Yorimitsu, H., Science of Synthesis Knowledge Updates, (2010) 3, 7.