P?P Condensation and P?N/P?P Bond Metathesis: Facile Synthesis of Cationic Tri‐ and Tetraphosphanes

Taube Clemens; Schwedtmann Kai; Noikham Medena; Somsook Ekasith; Hennersdorf Felix; Wolf Robert; Weigand Jan J.

摘要

Abstract > [L <sub>C</sub> R P((PhP) <sub>2</sub> C <sub>2</sub> H <sub>4</sub> )][OTf] ( 4?a,b [OTf]) and [L <sub>C</sub> iPr P(PPh <sub>2</sub> ) <sub>2</sub> ][OTf] ( 5?b [OTf]) were prepared from the reaction of imidazoliumyl‐substituted dipyrazolylphosphane triflate salts [L <sub>C</sub> R P(pyr) <sub>2</sub> ][OTf] ( 3?a,b [OTf]; a : R=Me, b =iPr; L <sub>C</sub> R =1,3‐dialkyl‐4,5‐dimethylimidazol‐2‐yl; pyr=3,5‐dimethylpyrazol‐1‐yl) with the secondary phosphanes PhP(H)C <sub>2</sub> H <sub>4</sub> P(H)Ph) and Ph <sub>2</sub> PH. A stepwise double P?N/P?P bond metathesis to catena‐tetraphosphane‐2,3‐diium triflate salt [(Ph <sub>2</sub> P) <sub>2</sub> (L <sub>C</sub> Me P) <sub>2</sub> ][OTf] <sub>2</sub> ( 7?a [OTf] <sub>2</sub> ) is observed when reacting 3?a [OTf] with diphosphane P <sub>2</sub> Ph <sub>4</sub> . The coordination ability of 5?b [OTf] was probed with selected coinage metal salts [Cu(CH <sub>3</sub> CN) <sub>4</sub> ]OTf, AgOTf and AuCl(tht) (tht=tetrahydrothiophene). For AuCl(tht), the helical complex [{(Ph <sub>2</sub> PPL <sub>C</sub> iPr )Au} <sub>4</sub> ][OTf] <sub>4</sub> ( 9 [OTf] <sub>4</sub> ) was unexpectedly formed as a result of a chloride‐induced P?P bond cleavage. The weakly coordinating triflate anion enables the formation of the expected copper(I) and silver(I) complexes [( 5?b )M(CH <sub>3</sub> CN) <sub>3</sub> ][OTf] <sub>2</sub> (M=Cu, Ag) ( 10 [OTf] <sub>2</sub> , 11 [OTf] <sub>2</sub> ). </abstract> </span> <span class="z_kbtn z_kbtnclass hoverxs" style="display: none;">展开▼</span> </div> <div class="translation abstracttxt"> <span class="zhankaihshouqi fivelineshidden" id="abstract"> <span>机译：</span><Abstract Type =“Main”XML：Lang =“en”> <标题类型=“main”>抽象</ title> > [L. <sub> c </ sub> r </ sup> p（（PHP） <sub> 2 </ sub> C <sub> 2 </ sub> H <sub> 4 </ sub> ）] [otf]（ 4？a，b </ b> [otf]）和[l <sub> c </ sub> ipr </ sup> P（PPH. <sub> 2 </ sub> 的） <sub> 2 </ sub> ] [otf]（ 5？b </ b> [otf]由咪唑鎓鎓取代的双唑烷基膦十三盐的反应制备[L <sub> c </ sub> r </ sup> P（Pyr） <sub> 2 </ sub> ] [otf]（ 3？a，b </ b> [otf]; a </ b> ：r =我， b </ b> = IPR; L. <sub> c </ sub> r </ sup> = 1,3-二烷基-4,5-二甲基咪唑-2-基;用二次磷酸pHP（H）C的Pyr = 3,5-二甲基吡唑-1-基 <sub> 2 </ sub> H <sub> 4 </ sub> p（h）pH）和pH <sub> 2 </ sub> pH。逐步双p？n / p？p粘合到Catena-tarphane-2,3-硫化物盐[（pH） <sub> 2 </ sub> P） <sub> 2 </ sub> （L. <sub> c </ sub> me </ sup> P） <sub> 2 </ sub> ] [otf] <sub> 2 </ sub> （ 7？a </ b> [otf] <sub> 2 </ sub> 在反应时观察到） 3？a </ b> 用二磷酸p <sub> 2 </ sub> 博士 <sub> 4 </ sub> 。协调能力 5？b </ b> 用选定的凝固金属盐探测[otf]（CH <sub> 3 </ sub> CN） <sub> 4 </ sub> ] OTF，agotf和AuCl（THT）（THT =四氢噻吩）。对于AUCL（THT），螺旋复合物[{（pH <sub> 2 </ sub> PPL. <sub> c </ sub> ipr </ sup> ）au} <sub> 4 </ sub> ] [otf] <sub> 4 </ sub> （ 9 </ b> [otf] <sub> 4 </ sub> ）由于氯化物诱导的p≤P粘结切割而出乎意料地形成。弱协调的Triflate阴离子使得能够形成预期的铜（I）和银（I）复合物[（ 5？b </ b> ）m（ch <sub> 3 </ sub> CN） <sub> 3 </ sub> ] [otf] <sub> 2 </ sub> （m = Cu，Ag）（ 10 </ b> [otf] <sub> 2 </ sub> 那 11 </ b> [otf] <sub> 2 </ sub> ）。 </ p> </摘要> </span> <span class="z_kbtn z_kbtnclass hoverxs" style="display: none;">展开▼</span> </div> </div> <div class="record"> <h2 class="all_title" id="enpatent33" >著录项</h2> <ul> <li> <span class="lefttit">来源</span> <div style="width: 86%;vertical-align: text-top;display: inline-block;"> <a href='/journal-foreign-19011/'>《Angewandte Chemie》</a> <b style="margin: 0 2px;">|</b><span>2020年第9期</span><b style="margin: 0 2px;">|</b><span>共7页</span> </div> </li> <li> <div class="author"> <span class="lefttit">作者</span> <p id="fAuthorthree" class="threelineshidden zhankaihshouqi"> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Taube Clemens&option=202" target="_blank" rel="nofollow">Taube Clemens;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Schwedtmann Kai&option=202" target="_blank" rel="nofollow">Schwedtmann Kai;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Noikham Medena&option=202" target="_blank" rel="nofollow">Noikham Medena;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Somsook Ekasith&option=202" target="_blank" rel="nofollow">Somsook Ekasith;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Hennersdorf Felix&option=202" target="_blank" rel="nofollow">Hennersdorf Felix;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Wolf Robert&option=202" target="_blank" rel="nofollow">Wolf Robert;</a> <a href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=Weigand Jan J.&option=202" target="_blank" rel="nofollow">Weigand Jan J.;</a> </p> <span class="z_kbtnclass z_kbtnclassall hoverxs" id="zkzz" style="display: none;">展开▼</span> </div> </li> <li> <div style="display: flex;"> <span class="lefttit">作者单位</span> <div style="position: relative;margin-left: 3px;max-width: 639px;"> <div class="threelineshidden zhankaihshouqi" id="fOrgthree"> <p>Faculty of Chemistry and Food ChemistryTechnische Universit?t Dresden01062 Dresden Germany;</p> <p>Faculty of Chemistry and Food ChemistryTechnische Universit?t Dresden01062 Dresden Germany;</p> <p>Department of ChemistryMahidol University272 Tungphayathai Rama 6 Road Rachathewi Bangkok 10400 Thailand;</p> <p>Department of ChemistryMahidol University272 Tungphayathai Rama 6 Road Rachathewi Bangkok 10400 Thailand;</p> <p>Faculty of Chemistry and Food ChemistryTechnische Universit?t Dresden01062 Dresden Germany;</p> <p>Institute of Inorganic ChemistryUniversit?t Regensburg93040 Regensburg Germany;</p> <p>Faculty of Chemistry and Food ChemistryTechnische Universit?t Dresden01062 Dresden Germany;</p> </div> <span class="z_kbtnclass z_kbtnclassall hoverxs" id="zhdw" style="display: none;">展开▼</span> </div> </div> </li> <li > <span class="lefttit">收录信息</span> <span style="width: 86%;vertical-align: text-top;display: inline-block;"></span> </li> <li> <span class="lefttit">原文格式</span> <span>PDF</span> </li> <li> <span class="lefttit">正文语种</span> <span>eng</span> </li> <li> <span class="lefttit">中图分类</span> <span><a href="https://www.zhangqiaokeyan.com/clc/1188.html" title="应用化学">应用化学;</a></span> </li> <li class="antistop"> <span class="lefttit">关键词</span> <p style="width: 86%;vertical-align: text-top;"> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=cationic polyphosphanes&option=203" rel="nofollow">cationic polyphosphanes;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=gold complex&option=203" rel="nofollow">gold complex;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=phosphorus ligands&option=203" rel="nofollow">phosphorus ligands;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=P?P bond metathesis&option=203" rel="nofollow">P?P bond metathesis;</a> <a style="color: #3E7FEB;" href="/search.html?doctypes=4_5_6_1-0_4-0_1_2_3_7_9&sertext=reductive coupling&option=203" rel="nofollow">reductive coupling;</a> </p> <div class="translation"> 机译：阳离子聚膦;金色复合物;磷配体;p？p键复位;还原耦合; </div> </li> </ul> </div> </div> <div class="literature cardcommon"> <div class="similarity "> <h3 class="all_title" id="enpatent66">相似文献</h3> <div class="similaritytab clearfix"> 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