Tricarbonyl(1,3-diphosphaallyl)cobalt, a Phosphorus Analogue of (η3-Allyl)tricarbonylcobalt

✍ Scribed by Prof. Dr. Rolf Appel; Winfried Schuhn; Dr. Falk Knoch

• Publisher: John Wiley and Sons
• Year: 1985
• Tongue: English
• Weight: 222 KB
• Volume: 24
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.198504201

✦ Synopsis

R-XC1, + 3 C(SilLle,), 7 R-X 3 LlCl v c1' -CI,C(SiMe,)> C(SiMe3)2 l a -c 2 3 a -c 4 c

(20.6 g, 0.09 mol) cooled to -110°C. The mixture was stirred for 3 h, then treated with a solution of l c (6.57 g, 0.03 mol) in T H F (10 mL), and allowed to warm to -15°C. The solvents were then removed and the mixture was taken up in SO mL of pre-cooled pentane and filtered. Finally, solvent and dichlorohis(trimethyIsi)yl)methane were condensed off as quickly as possible at room temperature in a vacuum. From the solution of the residue in 10 mL pentane, 3c precipitated as a red solid. At room temperature. 3c undergoes complete conversion within I2 h into 4c, which can be recrystallized from pentane. M.p. 91°C (4c), yield 67%.