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An Organotin Route for the Preparation of 2,6-Bis(diphenylphosphino)bromo-benzene and the Related Bis(Phosphine Oxide). Precursors for Novel Ligands
Zeitschrift für anorganische und allgemeine Chemie ( IF 1.1 ) Pub Date : 2021-07-23 , DOI: 10.1002/zaac.202100210 Fabio Meyer 1 , Thomas Kuzmera 1 , Enno Lork 1 , Matthias Vogt 1 , Jens Beckmann 2
Zeitschrift für anorganische und allgemeine Chemie ( IF 1.1 ) Pub Date : 2021-07-23 , DOI: 10.1002/zaac.202100210 Fabio Meyer 1 , Thomas Kuzmera 1 , Enno Lork 1 , Matthias Vogt 1 , Jens Beckmann 2
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The 2,6-difluorophenyltrialkylstannanes 2,6-F2C6H3SnR3 (1, R=Me; 2, R=Bu) were prepared from commercial products. With Ph2PLi, 1 and 2 underwent nucleophilic substitution to give the 2,6-bis(diphenylphosphino)phenyltrialkylstannanes 2,6-(Ph2P)2C6H3SnR3 (3, R=Me; 4, R=Bu). The reaction of 3 with n-BuLi and BrCH2CH2Br afforded 2,6-bis(diphenylphosphino)bromobenzene (2,6-(Ph2P)2C6H3Br, 5), the oxidation of which gave the related bis(phosphine oxide) 2,6-[Ph2P(O)]2C6H3Br (6). The reaction of 5 with n-BuLi gave rise to the formation of 2,6-bis(diphenylphosphino)phenyl lithium, 2,6-(Ph2P)2C6H3Li (7). Attempts to prepare the related bis(phosphine oxide) 2,6-[Ph2P(O)]2C6H3Li (8) from 6 in a similar way at low temperatures was hampered by decomposition. Compounds 3, 5 and 7 hold potential for a new anionic tridentate PCP−coordinating ligand, namely, the bis(2,6-diphenyl)phosphinophenyl ion [2,6-(Ph2P)2C6H3]−.
中文翻译：
用于制备 2,6-双（二苯基膦）溴苯和相关双（氧化膦）的有机锡路线。新型配体的前体
2,6-二氟苯基三烷基锡烷2,6-F 2 C 6 H 3 SnR 3 ( 1，R=Me；2，R=Bu)由商业产品制备。使用Ph 2 PLi，1和2进行亲核取代得到2,6-双(二苯基膦基)苯基三烷基锡烷2,6-(Ph 2 P) 2 C 6 H 3 SnR 3 ( 3 , R=Me; 4 , R=卜）。的反应3与Ñ正丁基锂和BRCH 2 CH 2Br得到2,6-双(二苯基膦基)溴苯(2,6-(Ph 2 P) 2 C 6 H 3 Br, 5 )，其氧化得到相关的双(氧化膦) 2,6-[Ph 2 P(O)] 2 C 6 H 3 Br ( 6 )。5与n- BuLi反应生成 2,6-双(二苯基膦基)苯基锂、2,6-(Ph 2 P) 2 C 6 H 3 Li ( 7 )。尝试制备相关的双（氧化膦）2,6-[Ph 2 P(O)] 2来自6 的C 6 H 3 Li ( 8 )在低温下以类似的方式受到分解的阻碍。化合物3，5和7保持潜在的新阴离子三齿PCP-的配位体，即二（2,6-二苯基）phosphinophenyl离子[2,6-（PH 2 P）2 C ^ 6 ħ 3 ] - 。
更新日期：2021-10-01
中文翻译：
用于制备 2,6-双（二苯基膦）溴苯和相关双（氧化膦）的有机锡路线。新型配体的前体
2,6-二氟苯基三烷基锡烷2,6-F 2 C 6 H 3 SnR 3 ( 1，R=Me；2，R=Bu)由商业产品制备。使用Ph 2 PLi，1和2进行亲核取代得到2,6-双(二苯基膦基)苯基三烷基锡烷2,6-(Ph 2 P) 2 C 6 H 3 SnR 3 ( 3 , R=Me; 4 , R=卜）。的反应3与Ñ正丁基锂和BRCH 2 CH 2Br得到2,6-双(二苯基膦基)溴苯(2,6-(Ph 2 P) 2 C 6 H 3 Br, 5 )，其氧化得到相关的双(氧化膦) 2,6-[Ph 2 P(O)] 2 C 6 H 3 Br ( 6 )。5与n- BuLi反应生成 2,6-双(二苯基膦基)苯基锂、2,6-(Ph 2 P) 2 C 6 H 3 Li ( 7 )。尝试制备相关的双（氧化膦）2,6-[Ph 2 P(O)] 2来自6 的C 6 H 3 Li ( 8 )在低温下以类似的方式受到分解的阻碍。化合物3，5和7保持潜在的新阴离子三齿PCP-的配位体，即二（2,6-二苯基）phosphinophenyl离子[2,6-（PH 2 P）2 C ^ 6 ħ 3 ] - 。
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