Synthesis of Boryl Metal Complexes with Additional Agostic Stabilization by Hydroboration of Fischer Carbyne Complexes

✍ Scribed by Priv.-Doz. Dr. Hubert Wadepohl; Dipl.-Chem. Ulrich Arnold; Dr. Hans Pritzkow

• Book ID: 101560038
• Publisher: John Wiley and Sons
• Year: 1997
• Tongue: English
• Weight: 424 KB
• Volume: 36
• Category: Article
• ISSN: 0044-8249
• DOI: 10.1002/anie.199709741

✦ Synopsis

Typical synthesis procedure: Tetraethyldiborane (310 mg, 4.43 mmol hydride)[281 was added to 4b (530 mg, 0.83 mmol) [27] in toluene (20 mL). The mixture was heated to 60°C for 15 min (color change to yellow). After cooling, the solution was concentrated under vacuum and allowed to crystallize at -20 "C. The microcrystailine precipitate was dissolved in a small volume of toluene and chromatographed on a silica column with toluene at -45 "C. The solvent was removed from the eluate under reduced pressure, the residue washed several times with pentane, and then dried under vacuum. Yield 380 mg (67%) of pale yellow powder. Correct C,H,N analysis.