Yang Ying, Schulz Thomas, John Michael, Ringe Arne, Roesky Herbert W, Stalke Dietmar, Magull Jörg, Ye Hongqi
School of Chemistry and Chemical Engineering, Central South University, 410083 Changsha, People's Republic of China.
Inorg Chem. 2008 Apr 7;47(7):2585-92. doi: 10.1021/ic701896r. Epub 2008 Mar 4.
Monomeric aluminum chloride amides with the general formula LAl(Cl)NR2 (1, R = Me; 2, R = iPr; 3, R = SiMe 3; L = HC[C(Me)N(Ar)]2; Ar = 2,6- iPr2C6H3) were prepared by selected routes. Treatment of LAlBr 2 (4) and LAlI2 with LiNMe2 yielded LAl(Br)NMe2 (5) and LAl(I)NMe2 (6), respectively. The alkylation of 1 and 2 with MeLi gave the corresponding methylated compounds LAl(Me)NR2 (7, R = Me; 8, R = iPr); however, no reaction of 3 with MeLi was observed because of steric hindrance. Subsequent fluorination of 1- 3 afforded LAl(F)NR2 (9, R = Me; 10, R = iPr; 11, R = SiMe3). Compounds 1-11 were characterized by multinuclear NMR, electron impact mass spectrometry, and IR. The constitution of compounds 1-3 was confirmed by single-crystal X-ray diffraction studies.
通过特定路线制备了通式为LAl(Cl)NR₂（1，R = 甲基；2，R = 异丙基；3，R = 三甲基硅基；L = HC[C(甲基)N(芳基)]₂；芳基 = 2,6 - 二异丙基苯基）的单体氯化铝酰胺。用LiNMe₂处理LAlBr₂（4）和LAlI₂分别得到LAl(Br)NMe₂（5）和LAl(I)NMe₂（6）。用甲基锂对1和2进行烷基化反应得到相应的甲基化化合物LAl(甲基)NR₂（7，R = 甲基；8，R = 异丙基）；然而，由于空间位阻，未观察到3与甲基锂发生反应。随后对1 - 3进行氟化得到LAl(F)NR₂（9，R = 甲基；10，R = 异丙基；11，R = 三甲基硅基）。通过多核核磁共振、电子轰击质谱和红外光谱对化合物1 - 11进行了表征。通过单晶X射线衍射研究证实了化合物1 - 3的结构。
