M. V. Moskalev, A. A. Skatova, A. A. Bazanov, E. V. Baranov, I. L. Fedushkin
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The reaction of <b>I</b> with BH<sub>3</sub>∙SMe<sub>2</sub> (1 : 1) in toluene affords the product of hydroboration of one formate group [(Ar<sup>BIG</sup>-bian)Al(μ-OC(H)O)(OB(H)OCH<sub>3</sub>)Li(Thf)]<sub>2</sub> (<b>II</b>), while the reaction of <b>I</b> with BH<sub>3</sub>∙SMe<sub>2</sub> (1 : 2) is accompanied by reduction of both formate groups and gives complex [(Ar<sup>BIG</sup>-bian)Al(OBOCH<sub>3</sub>)<sub>2</sub>OLi<sub>2</sub>(Thf)<sub>2</sub>BH<sub>4</sub>]<sub>2</sub> (<b>III</b>), methoxyboroxine (CH<sub>3</sub>OBO)<sub>3</sub> and, presumably, compound [(Ar<sup>BIG</sup>-bian)AlOCH<sub>3</sub>]. The reaction of <b>I</b> with one equivalent of ammonia in THF gives adduct [(Ar<sup>BIG</sup>-bian)Al(NH<sub>3</sub>)(μ-OC(H)O)<sub>2</sub>Li(Thf)<sub>2</sub>] (<b>IV</b>), in which ammonia is coordinated to the aluminum atom, while the key bonds in <b>I</b> have not undergone ammonolysis. Compounds <b>II</b>–<b>IV</b> were characterized by IR and NMR spectroscopy, elemental analysis, and X-ray diffraction (CCDC no. 2255017 (<b>II</b>), 2255018 (<b>III</b>), 2255019 (<b>IV</b>)).</p>","PeriodicalId":1,"journal":{"name":"Accounts of Chemical Research","volume":null,"pages":null},"PeriodicalIF":16.4000,"publicationDate":"2024-05-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Reactions of Carbon Dioxide Bound to Aluminum Diimine Hydride with Borane Dimethyl Sulfide and Ammonia\",\"authors\":\"M. V. Moskalev, A. A. Skatova, A. A. Bazanov, E. V. Baranov, I. L. Fedushkin\",\"doi\":\"10.1134/S1070328423600936\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>The reaction of aluminum bis-formate acenaphthene-1,2-diimine complex [(Ar<sup>BIG</sup>-bian)Al(μ-OC(H)O)<sub>2</sub>Li(Thf)<sub>2</sub>] (<b>I</b>) (Ar<sup>BIG</sup>-bian = 1,2-bis[(2,6-dibenzhydryl-4-methylphenyl)imino]acenaphthene), prepared by binding carbon dioxide by aluminum diimine hydride [(Ar<sup>BIG</sup>-bian)Al(H)<sub>2</sub>]<sup>–</sup>[Li(Thf)<sub>4</sub>]<sup>+</sup>, with borane dimethyl sulfide and ammonia was studied. The reaction of <b>I</b> with BH<sub>3</sub>∙SMe<sub>2</sub> (1 : 1) in toluene affords the product of hydroboration of one formate group [(Ar<sup>BIG</sup>-bian)Al(μ-OC(H)O)(OB(H)OCH<sub>3</sub>)Li(Thf)]<sub>2</sub> (<b>II</b>), while the reaction of <b>I</b> with BH<sub>3</sub>∙SMe<sub>2</sub> (1 : 2) is accompanied by reduction of both formate groups and gives complex [(Ar<sup>BIG</sup>-bian)Al(OBOCH<sub>3</sub>)<sub>2</sub>OLi<sub>2</sub>(Thf)<sub>2</sub>BH<sub>4</sub>]<sub>2</sub> (<b>III</b>), methoxyboroxine (CH<sub>3</sub>OBO)<sub>3</sub> and, presumably, compound [(Ar<sup>BIG</sup>-bian)AlOCH<sub>3</sub>]. The reaction of <b>I</b> with one equivalent of ammonia in THF gives adduct [(Ar<sup>BIG</sup>-bian)Al(NH<sub>3</sub>)(μ-OC(H)O)<sub>2</sub>Li(Thf)<sub>2</sub>] (<b>IV</b>), in which ammonia is coordinated to the aluminum atom, while the key bonds in <b>I</b> have not undergone ammonolysis. 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引用次数: 0
摘要
AbstractThe reaction of aluminum bis-formate acenaphthene-1,2-diimine complex [(ArBIG-bian)Al(μ-OC(H)O)2Li(Thf)2] (I) (ArBIG-bian = 1,2-bis[(2,6-dibenzhydryl-4-methylphenyl)imino]acenaphthene)、研究了由二亚胺氢化铝[(ArBIG-bian)Al(H)2]-[Li(Thf)4]+ 与硼烷二甲基硫醚和氨结合制备的二氧化碳。I 与 BH3∙SMe2 (1 : 1) 在甲苯中反应生成了一个甲酸基团的硼氢化产物 [(ArBIG-bian)Al(μ-OC(H)O)(OB(H)OCH3)Li(Thf)]2（II），而 I 与 BH3∙SMe2 (1 ：2）的反应伴随着两个甲酸基团的还原，并得到复合物[(ArBIG-bian)Al(OBOCH3)2OLi2(Thf)2BH4]2（III）、甲氧基硼氧烷（CH3OBO）3 以及可能的化合物[(ArBIG-bian)AlOCH3]。I 与一当量的氨在 THF 中反应生成加合物[(ArBIG-bian)Al(NH3)(μ-OC(H)O)2Li(Thf)2]（IV），其中氨与铝原子配位，而 I 中的关键键没有发生氨解作用。化合物 II-IV 的特征采用了红外光谱、核磁共振光谱、元素分析和 X 射线衍射（CCDC 编号：2255017 (II)、2255018 (III)、2255019 (IV)）。
Reactions of Carbon Dioxide Bound to Aluminum Diimine Hydride with Borane Dimethyl Sulfide and Ammonia
The reaction of aluminum bis-formate acenaphthene-1,2-diimine complex [(ArBIG-bian)Al(μ-OC(H)O)2Li(Thf)2] (I) (ArBIG-bian = 1,2-bis[(2,6-dibenzhydryl-4-methylphenyl)imino]acenaphthene), prepared by binding carbon dioxide by aluminum diimine hydride [(ArBIG-bian)Al(H)2]–[Li(Thf)4]+, with borane dimethyl sulfide and ammonia was studied. The reaction of I with BH3∙SMe2 (1 : 1) in toluene affords the product of hydroboration of one formate group [(ArBIG-bian)Al(μ-OC(H)O)(OB(H)OCH3)Li(Thf)]2 (II), while the reaction of I with BH3∙SMe2 (1 : 2) is accompanied by reduction of both formate groups and gives complex [(ArBIG-bian)Al(OBOCH3)2OLi2(Thf)2BH4]2 (III), methoxyboroxine (CH3OBO)3 and, presumably, compound [(ArBIG-bian)AlOCH3]. The reaction of I with one equivalent of ammonia in THF gives adduct [(ArBIG-bian)Al(NH3)(μ-OC(H)O)2Li(Thf)2] (IV), in which ammonia is coordinated to the aluminum atom, while the key bonds in I have not undergone ammonolysis. Compounds II–IV were characterized by IR and NMR spectroscopy, elemental analysis, and X-ray diffraction (CCDC no. 2255017 (II), 2255018 (III), 2255019 (IV)).
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