Trimethylamine N-oxide promoted decarbonylation reactions of molybdenum and tungsten hexacarbonyls with dimethylglyoxime

A. Abubakar, U. Eke
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Abstract

Decarbonylation of Mo and W hexacarbonyls in the presence of dimethylglyoxime was carried out under the control of trimethylamine N-oxide (TMNO). The two DMG substituted carbonyl complexes were prepared in a one pot synthesis using manipulated Schlenk techniques under dinitrogen in tetrahydrofuran. The Mo complex system was successfully carried out by stirring the mixture of the molybdenum hexacarbonyl and DMG in tetrahydrofuran at room temperature for 18hrs. A similar procedure afforded the starting ligand material for the W complex analogue. However, further refluxing for 6 h gave the desired W complex. The complexes were characterized using 1 H NMR, IR, and CHN analyses. Results showed that the reactions produced analytically pure, mono-product dicarbonyl species; Mo(CO) 2 (DMG) 2 I and W(CO) 2 (DMG) 2 II where two DMG moieties were coordinated to the central metal atom through one N and O atoms respectively of each of the oxime groups. Keywords: Bioorganometallic, Metal carbonyl, CO-RMs, Decarbonylation, Trimethylamine N-oxide
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三甲胺n -氧化物促进钼、钨六羰基与二甲基乙氧肟的脱羰反应
在三甲胺n -氧化物(TMNO)的控制下,Mo和W六羰基在二甲基乙肟存在下进行了脱碳反应。以四氢呋喃为溶剂,在二氮条件下,采用操纵Schlenk技术,一锅法合成了两种DMG取代羰基配合物。将六羰基钼和DMG的混合物在四氢呋喃中室温搅拌18h,成功地制备了Mo配合物体系。类似的过程为W络合物类似物提供了起始配体材料。然而,进一步回流6小时得到所需的W复合物。通过1h NMR, IR和CHN分析对配合物进行了表征。结果表明,该反应产生了纯的单产物二羰基物质;Mo(CO) 2 (DMG) 2 I和W(CO) 2 (DMG) 2 II,其中两个DMG基团分别通过每个肟基的一个N和O原子与中心金属原子配位。关键词:生物有机金属,金属羰基,CO-RMs,脱羰,三甲胺n -氧化物
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